data_ras1306_squeeze
_audit_creation_date "13-09-02"
_audit_creation_method CRYSTALS_ver_14.40
_audit_update_record
;
2013-09-03 - Report on C20 H32 Cl6 Cu4 N8 O
by Anthony C. Willis
for Rasoul Vafazadeh
2013-09-03 - passes checkcif tests with minor warnings
;
_oxford_structure_analysis_title 'ras1306 At 16:17 on 29/ 8'
_chemical_name_systematic ?
_chemical_melting_point ?
_cell_length_a 13.3604(3)
_cell_length_b 8.8530(1)
_cell_length_c 16.6709(4)
_cell_angle_alpha 90
_cell_angle_beta 95.0682(9)
_cell_angle_gamma 90
_cell_volume 1964.12(7)
_symmetry_cell_setting 'monoclinic'
_symmetry_space_group_name_H-M 'P 1 2/n 1 '
_symmetry_space_group_name_Hall '-P 2yac '
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,-y,-z'
'-x+1/2,y,-z+1/2'
'x+1/2,-y,z+1/2'
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687
0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424
0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194
1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu 0.3201 1.2651 13.3380 3.5828 7.1676 0.2470 5.6158 11.3966
1.6735 64.8126 1.1910 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975
1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239
0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
_cell_formula_units_Z 2
# Given Formula = C25 H40 Cl6 Cu4 N10 O1
# Dc = 1.63 Fooo = 868.00 Mu = 25.79 M = 481.78
# Found Formula = C20 H32 Cl6 Cu4 N8 O1
# Dc = 1.47 FOOO = 868.00 Mu = 25.69 M = 433.71
_chemical_formula_sum 'C20 H32 Cl6 Cu4 N8 O'
_chemical_formula_moiety 'C20 H32 Cl6 Cu4 N8 O'
_chemical_compound_source ' Yazd University '
_chemical_formula_weight 867.43
_cell_measurement_reflns_used 41891
_cell_measurement_theta_min 2.6
_cell_measurement_theta_max 27.5
_cell_measurement_temperature 200
_exptl_crystal_description 'rod'
_exptl_crystal_colour 'brown'
_exptl_crystal_size_min 0.070
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_max 0.440
_exptl_crystal_density_diffrn 1.467
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 868
_exptl_absorpt_coefficient_mu 2.569
# Sheldrick geometric approximatio 0.77 0.84
# Absorption correction
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.180
0 -1 0 0.260
1 0 1 0.030
-1 0 -1 0.040
-1 0 1 0.070
1 0 -1 0.030
_exptl_absorpt_correction_type 'integration'
_exptl_absorpt_correction_T_min 0.503
_exptl_absorpt_correction_T_max 0.848
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
#_diffrn_reflns_av_R_equivalents 0.038
# For a Kappa CCD, set Tmin to 1.0 and
# Tmax to the ratio of max:min frame scales in scale_all.log
_diffrn_measurement_device_type 'Nonius KappaCCD'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method ' \f and \w scans with CCD '
_diffrn_special_details
;
CCD data collecting conditions-
phi and omega scans of width 1.4 deg at rate 126 sec/frame
and at 12.6 sewc/frame,
crystal-detector distance 40mm,
multiple scan sets so over 95 percent of data collected with 4-fold
redundancy or more.
;
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'COLLECT (Nonius, 2001).'
_computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement
;
CRYSTALS (Betteridge et al., 2003),
SQUEEZE (Sluis, P. van der and Spek, A.L., 1990)
;
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics
;
ORTEP-II (Johnson 1976) in teXsan (MSC, 1992-1997)
;
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 200
_diffrn_reflns_number 37406
_reflns_number_total 4523
_diffrn_reflns_av_R_equivalents 0.049
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 4523
# Theoretical number of reflections is about 9029
_diffrn_reflns_theta_min 2.607
_diffrn_reflns_theta_max 27.505
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 27.505
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_h_max 17
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_limit_l_max 20
_reflns_limit_h_min -17
_reflns_limit_h_max 17
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 21
_oxford_diffrn_Wilson_B_factor 3.10
_oxford_diffrn_Wilson_scale 4.13
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_diff_density_min -0.99
_refine_diff_density_max 1.61
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.250 0.070 0.250 229 32 ' '
2 0.250 -0.096 0.750 229 32 ' '
_platon_squeeze_details
;
A region of disordered solvate molecules was identified
about a 2-fold axis.
;
# The current dictionary definitions do not cover the
# situation where the reflections used for refinement were
# selected by a user-defined sigma threshold
# The values actually used during refinement
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns 4519
_refine_ls_number_restraints 0
_refine_ls_number_parameters 182
_oxford_refine_ls_R_factor_ref 0.0473
_refine_ls_wR_factor_ref 0.1077
_refine_ls_goodness_of_fit_ref 1.0012
_refine_ls_shift/su_max 0.0018978
_refine_ls_shift/su_mean 0.0003376
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 4519
_refine_ls_R_factor_all 0.0473
_refine_ls_wR_factor_all 0.1077
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 4041
_refine_ls_R_factor_gt 0.0426
_refine_ls_wR_factor_gt 0.1052
# choose from: rm (reference molecule of known chirality),
# ad (anomolous dispersion - Flack), rmad (rm and ad),
# syn (from synthesis), unk (unknown) or . (not applicable).
_chemical_absolute_configuration '.'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_hydrogen_treatment constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[\s^2^(F^2^) + ( 0.04P)^2^ + 5.02P]
,where P=(max(Fo^2^,0) + 2Fc^2^)/3
;
# 1. SUBMISSION DETAILS
_publ_requested_journal ' test '
_publ_requested_category fm
_publ_contact_author_name ' Anthony C. Willis '
_publ_contact_author_address
;
Research School of Chemistry,
Australian National University,
Canberra, A. C. T. 0200, Australia
;
_publ_contact_letter
;
ENTER TEXT OF LETTER
;
_publ_requested_coeditor_name ?
_publ_contact_author_phone ' 61 2 6125 4109 '
_publ_contact_author_fax ' 61 2 6125 0750 '
_publ_contact_author_email ' willis@rsc.anu.edu.au '
#=============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic ?
_journal_date_to_coeditor ?
_journal_date_from_coeditor ?
_journal_date_accepted ?
_journal_date_printers_first ?
_journal_date_printers_final ?
_journal_date_proofs_out ?
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code ?
_journal_coeditor_notes
;
?
;
_journal_techeditor_code ?
_journal_techeditor_notes
;
?
;
_journal_coden_ASTM ?
_journal_name_full ?
_journal_year ?
_journal_volume ?
_journal_issue ?
_journal_page_first ?
_journal_page_last ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#=============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
Crystal structure of
[Cu~4~Cl~6~O(C~5~H~8~N~2~)~4~]
--- ras1306a
;
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
loop_
_publ_author_name
_publ_author_address
'N. Hasanzadeh '
;
Department of Chemistry,
Yazd University,
Yazd, Iran
;
'Rasoul Vafazadeh '
;
Department of Chemistry,
Yazd University,
Yazd, Iran
;
' Anthony C. Willis '
;
Research School of Chemistry,
The Australian National University,
Canberra, A. C. T. 0200, Australia
;
#==============================================================================
# 4. TEXT
_publ_section_abstract #Text of the abstract
;
The crystal structure of
[Cu~4~Cl~6~O(C~5~H~8~N~2~)~4~]
is reported.
;
_publ_section_comment #Text of the paper
;
The crystallographic asymmetric unit consists of one-half of a
[Cu~4~Cl~6~O(C~5~H~8~N~2~)~4~]
molecule.
The other half of the molecule is generated by a crystallographic
two-fold symmetry operation.
The atom site Cl(4) has an occupancy of 0.5 and is situated
close to the two-fold axis. Sites Cl(4) and
Cl(4)(1-x,y,1.5-z) at too close together (1.786(6)\%A)
to be simultaneously occupied.
The central atom in the cluster is assumed to be an oxygen
atom on account of the satisfactory refinement of
its displacement parameters.
There was a region of disordered solvate in the structure
which could not be satisfactorily modelled.
The surface of the crystals supplied looked pitted, consistent
with loss of solvate after removal from the supernatant
used in crystallization.
The electron density in this part of the structure
has been removed using the utility SQUEEZE
[Sluis, P. van der and Spek, A.L. (1990)].
;
_publ_section_acknowledgements # Acknowledgments
;
;
_publ_section_figure_captions #Captions to figures
;
?
;
_publ_section_exptl_refinement
# see also _refine_ls_hydrogen for refinement keywords.
;
;
_publ_section_exptl_prep
;
The compound was prepared by NH and RV
and was recrystallised from ???.
The sample identification was H10-new.
A previous sample, labelled H10, gave crystals with the same
unit cell and same structure.
;
_refine_special_details #Text of the paper
;
After location of the metallo-organic species,
a subsequent difference electron density map revealed
a number of peaks isolated from the principal molecule which
appeared to indicate the presence of a disordered solvate molecule.
The peaks formed a cyclic 5- or 6-membered species
with sites of occupancy <0.5.
No sensible disordered model could be
constructed which would match the observed peaks,
so the computer program SQUEEZE within PLATON
was used to account for the electron density in this region of the unit cell.
[Sluis, P. van der and Spek, A.L. (1990)
Acta Crystallogr., Sect. A, 46, 194-201.]
The program identified solvent accessible voids totalling 459.9\%A^3^,
and 64 electrons per unit cell were recovered.
The formula weight, density etc. listed in the Tables do not include any
correction for the missing solvate.
H atoms were added at calculated positions
and then were refined with soft restraints on the
bond lengths and angles to regularise their geometry
(C---H in the range 0.93--0.98\%A, N---H = 0.86\%A) and
U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom),
after which the positions were refined with riding constraints
and the displacement parameters were held fixed.
The largest peaks in the final difference electron density map
are located close to Cl atoms.
;
# Insert your own references if required - in alphabetical order
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, G., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435--?.
Betteridge, P. W., Carruthers, J. R., Cooper, R. I., Prout, K. & Watkin, D. J.
(2003). J. Appl. Cryst. 36, 1487--?.
Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands.
Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276,
edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326.
New York: Academic Press.
Molecular Structure Corporation. (1992-1997). teXsan.
Single Crystal Structure Analysis Software. Version 1.8.
MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA.
Johnson, C.K. (1976).
ORTEP-II, A Fortran Thermal-Ellipsoid Plot Program, Report ORNL-5138,
Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA.
;
# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3
# Replace last . with number of unfound hydrogen atoms attached to an atom.
# ..._refinement_flags_...
# . no refinement constraints S special position constraint on site
# G rigid group refinement of site R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond) P partial occupancy constraint
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Cu1 Cu 0.79414(3) 0.52824(4) 0.66564(2) 0.0362 1.0000 Uani . . . . . .
Cu2 Cu 0.63882(3) 0.28892(4) 0.70536(2) 0.0338 1.0000 Uani . . . . . .
Cl1 Cl 0.66587(8) 0.40808(15) 0.58272(6) 0.0624 1.0000 Uani . . . . . .
Cl2 Cl 0.54963(7) 0.39369(17) 0.80965(6) 0.0672 1.0000 Uani . . . . . .
Cl3 Cl 0.7500 0.07354(15) 0.7500 0.0599 1.0000 Uani S T . . . .
Cl4 Cl 0.8133(2) 0.7174(2) 0.77219(13) 0.0659 0.5000 Uani . . . . . .
O1 O 0.7500 0.4063(3) 0.7500 0.0302 1.0000 Uani S T . . . .
N1 N 0.8332(2) 0.6706(3) 0.58380(17) 0.0406 1.0000 Uani . . . . . .
N2 N 0.8304(2) 0.8221(3) 0.59501(18) 0.0430 1.0000 Uani . . . . . .
N3 N 0.5318(2) 0.1584(3) 0.65743(18) 0.0398 1.0000 Uani . . . . . .
N4 N 0.5451(2) 0.0073(3) 0.64978(19) 0.0441 1.0000 Uani . . . . . .
C1 C 0.8573(4) 1.0654(5) 0.5287(3) 0.0623 1.0000 Uani . . . . . .
C2 C 0.8559(3) 0.8981(4) 0.5306(2) 0.0450 1.0000 Uani . . . . . .
C3 C 0.8756(3) 0.7909(5) 0.4752(2) 0.0480 1.0000 Uani . . . . . .
C4 C 0.8606(2) 0.6496(4) 0.5096(2) 0.0395 1.0000 Uani . . . . . .
C5 C 0.8693(3) 0.4964(4) 0.4743(2) 0.0482 1.0000 Uani . . . . . .
C6 C 0.4049(3) 0.3483(6) 0.6103(3) 0.0700 1.0000 Uani . . . . . .
C7 C 0.4440(3) 0.1903(5) 0.6166(2) 0.0500 1.0000 Uani . . . . . .
C8 C 0.4021(3) 0.0576(6) 0.5838(3) 0.0608 1.0000 Uani . . . . . .
C9 C 0.4674(3) -0.0578(5) 0.6058(3) 0.0566 1.0000 Uani . . . . . .
C10 C 0.4632(5) -0.2236(6) 0.5923(4) 0.0865 1.0000 Uani . . . . . .
H11 H 0.8881 1.0997 0.4827 0.0935 1.0000 Uiso R . . . . .
H13 H 0.8938 1.1059 0.5754 0.0934 1.0000 Uiso R . . . . .
H12 H 0.7900 1.1042 0.5254 0.0934 1.0000 Uiso R . . . . .
H31 H 0.8974 0.8090 0.4238 0.0583 1.0000 Uiso R . . . . .
H52 H 0.9090 0.4981 0.4293 0.0719 1.0000 Uiso R . . . . .
H51 H 0.9005 0.4324 0.5161 0.0719 1.0000 Uiso R . . . . .
H53 H 0.8037 0.4566 0.4588 0.0720 1.0000 Uiso R . . . . .
H61 H 0.3379 0.3556 0.6245 0.1055 1.0000 Uiso R . . . . .
H63 H 0.4463 0.4143 0.6447 0.1052 1.0000 Uiso R . . . . .
H62 H 0.4072 0.3838 0.5569 0.1054 1.0000 Uiso R . . . . .
H81 H 0.3408 0.0476 0.5527 0.0734 1.0000 Uiso R . . . . .
H102 H 0.4252 -0.2445 0.5417 0.1301 1.0000 Uiso R . . . . .
H101 H 0.4321 -0.2725 0.6352 0.1301 1.0000 Uiso R . . . . .
H103 H 0.5310 -0.2620 0.5908 0.1298 1.0000 Uiso R . . . . .
H21 H 0.8171 0.8618 0.6382 0.0526 1.0000 Uiso R . . . . .
H41 H 0.5875 -0.0414 0.6796 0.0538 1.0000 Uiso R . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0486(2) 0.0289(2) 0.0316(2) 0.00278(15) 0.00711(16) -0.00165(16)
Cu2 0.0374(2) 0.0297(2) 0.0335(2) -0.00054(15) -0.00066(15) -0.00253(15)
Cl1 0.0536(5) 0.0960(8) 0.0358(4) 0.0184(5) -0.0068(4) -0.0197(6)
Cl2 0.0405(5) 0.1101(10) 0.0517(6) -0.0286(6) 0.0083(4) 0.0020(5)
Cl3 0.0581(8) 0.0317(6) 0.0843(11) 0.0000 -0.0257(7) 0.0000
Cl4 0.1196(19) 0.0319(8) 0.0514(11) -0.0120(8) 0.0379(12) -0.0241(10)
O1 0.0345(15) 0.0265(14) 0.0291(14) 0.0000 0.0013(11) 0.0000
N1 0.0499(17) 0.0341(14) 0.0384(15) 0.0034(12) 0.0075(12) -0.0031(12)
N2 0.0547(18) 0.0339(14) 0.0410(15) 0.0031(12) 0.0068(13) -0.0050(13)
N3 0.0409(15) 0.0372(15) 0.0402(15) 0.0001(12) -0.0037(12) -0.0040(12)
N4 0.0504(17) 0.0373(15) 0.0432(16) -0.0034(13) -0.0036(13) -0.0054(13)
C1 0.066(3) 0.044(2) 0.077(3) 0.015(2) 0.005(2) -0.012(2)
C2 0.0418(18) 0.0431(19) 0.050(2) 0.0110(16) 0.0008(15) -0.0089(15)
C3 0.048(2) 0.055(2) 0.0414(19) 0.0128(17) 0.0068(15) -0.0064(17)
C4 0.0351(16) 0.0473(19) 0.0361(16) 0.0036(15) 0.0033(13) -0.0044(14)
C5 0.051(2) 0.051(2) 0.044(2) -0.0020(16) 0.0103(16) 0.0003(17)
C6 0.052(2) 0.067(3) 0.088(4) 0.012(3) -0.014(2) 0.009(2)
C7 0.0405(19) 0.058(2) 0.050(2) 0.0046(18) -0.0062(16) -0.0053(17)
C8 0.050(2) 0.074(3) 0.055(2) -0.004(2) -0.0140(18) -0.015(2)
C9 0.064(3) 0.057(2) 0.048(2) -0.0106(19) -0.0003(18) -0.023(2)
C10 0.119(5) 0.059(3) 0.081(4) -0.021(3) 0.006(3) -0.037(3)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 0.5534(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 . Cu1 3_656 3.1447(8) yes
Cu1 . Cu2 3_656 3.0944(5) yes
Cu1 . Cl4 3_656 2.4908(19) yes
Cu1 . Cl2 3_656 2.4069(12) yes
Cu1 . Cu2 . 3.0783(6) yes
Cu1 . Cl1 . 2.3580(11) yes
Cu1 . Cl4 . 2.4386(19) yes
Cu1 . O1 . 1.9072(17) yes
Cu1 . N1 . 1.962(3) yes
Cu2 . Cu2 3_656 3.2030(8) yes
Cu2 . Cl1 . 2.3567(10) yes
Cu2 . Cl2 . 2.3810(10) yes
Cu2 . Cl3 . 2.4901(11) yes
Cu2 . O1 . 1.9091(16) yes
Cu2 . N3 . 1.953(3) yes
N1 . N2 . 1.355(4) yes
N1 . C4 . 1.334(4) yes
N2 . C2 . 1.337(5) yes
N2 . H21 . 0.834 no
N3 . N4 . 1.357(4) yes
N3 . C7 . 1.333(5) yes
N4 . C9 . 1.347(5) yes
N4 . H41 . 0.839 no
C1 . C2 . 1.482(5) yes
C1 . H11 . 0.953 no
C1 . H13 . 0.951 no
C1 . H12 . 0.959 no
C2 . C3 . 1.366(6) yes
C3 . C4 . 1.398(5) yes
C3 . H31 . 0.942 no
C4 . C5 . 1.487(5) yes
C5 . H52 . 0.956 no
C5 . H51 . 0.964 no
C5 . H53 . 0.959 no
C6 . C7 . 1.493(6) yes
C6 . H61 . 0.948 no
C6 . H63 . 0.959 no
C6 . H62 . 0.947 no
C7 . C8 . 1.392(6) yes
C8 . C9 . 1.372(7) yes
C8 . H81 . 0.935 no
C9 . C10 . 1.485(6) yes
C10 . H102 . 0.963 no
C10 . H101 . 0.961 no
C10 . H103 . 0.969 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cu1 3_656 Cu1 . Cu2 3_656 59.121(12) yes
Cu1 3_656 Cu1 . Cl4 3_656 49.63(4) yes
Cu2 3_656 Cu1 . Cl4 3_656 108.26(5) yes
Cu1 3_656 Cu1 . Cl2 3_656 103.59(3) yes
Cu2 3_656 Cu1 . Cl2 3_656 49.37(3) yes
Cl4 3_656 Cu1 . Cl2 3_656 141.69(7) yes
Cu1 3_656 Cu1 . Cu2 . 59.626(12) yes
Cu2 3_656 Cu1 . Cu2 . 62.516(15) yes
Cl4 3_656 Cu1 . Cu2 . 87.08(6) yes
Cl2 3_656 Cu1 . Cu2 . 102.32(3) yes
Cu1 3_656 Cu1 . Cl1 . 102.34(3) yes
Cu2 3_656 Cu1 . Cl1 . 104.43(3) yes
Cl4 3_656 Cu1 . Cl1 . 97.56(8) yes
Cl2 3_656 Cu1 . Cl1 . 116.83(5) yes
Cu2 . Cu1 . Cl1 . 49.22(3) yes
Cu1 3_656 Cu1 . Cl4 . 51.10(5) yes
Cu2 3_656 Cu1 . Cl4 . 87.63(6) yes
Cl4 3_656 Cu1 . Cl4 . 42.46(13) yes
Cl2 3_656 Cu1 . Cl4 . 100.46(8) yes
Cu2 . Cu1 . Cl4 . 110.21(5) yes
Cu1 3_656 Cu1 . O1 . 34.47(7) yes
Cu2 3_656 Cu1 . O1 . 35.84(4) yes
Cl4 3_656 Cu1 . O1 . 81.18(8) yes
Cl2 3_656 Cu1 . O1 . 85.05(5) yes
Cu2 . Cu1 . O1 . 36.25(4) yes
Cu1 3_656 Cu1 . N1 . 139.99(9) yes
Cu2 3_656 Cu1 . N1 . 147.64(9) yes
Cl4 3_656 Cu1 . N1 . 93.20(10) yes
Cl2 3_656 Cu1 . N1 . 99.03(9) yes
Cu2 . Cu1 . N1 . 144.86(9) yes
Cl1 . Cu1 . Cl4 . 139.55(8) yes
Cl1 . Cu1 . O1 . 85.46(4) yes
Cl4 . Cu1 . O1 . 82.59(8) yes
Cl1 . Cu1 . N1 . 96.12(9) yes
Cl4 . Cu1 . N1 . 92.75(10) yes
O1 . Cu1 . N1 . 174.33(11) yes
Cu2 3_656 Cu2 . Cu1 3_656 58.496(12) yes
Cu2 3_656 Cu2 . Cu1 . 58.988(12) yes
Cu1 3_656 Cu2 . Cu1 . 61.253(16) yes
Cu2 3_656 Cu2 . Cl1 . 101.31(3) yes
Cu1 3_656 Cu2 . Cl1 . 103.84(3) yes
Cu1 . Cu2 . Cl1 . 49.26(3) yes
Cu2 3_656 Cu2 . Cl2 . 99.45(3) yes
Cu1 3_656 Cu2 . Cl2 . 50.10(3) yes
Cu1 . Cu2 . Cl2 . 106.22(4) yes
Cl1 . Cu2 . Cl2 . 125.74(5) yes
Cu2 3_656 Cu2 . Cl3 . 49.97(2) yes
Cu1 3_656 Cu2 . Cl3 . 100.85(2) yes
Cu1 . Cu2 . Cl3 . 101.28(2) yes
Cl1 . Cu2 . Cl3 . 117.96(4) yes
Cl2 . Cu2 . Cl3 . 113.82(4) yes
Cu2 3_656 Cu2 . O1 . 32.98(7) yes
Cu1 3_656 Cu2 . O1 . 35.80(4) yes
Cu1 . Cu2 . O1 . 36.21(4) yes
Cl1 . Cu2 . O1 . 85.46(5) yes
Cl2 . Cu2 . O1 . 85.74(4) yes
Cu2 3_656 Cu2 . N3 . 143.65(9) yes
Cu1 3_656 Cu2 . N3 . 147.75(9) yes
Cu1 . Cu2 . N3 . 143.32(9) yes
Cl1 . Cu2 . N3 . 94.16(9) yes
Cl2 . Cu2 . N3 . 97.69(9) yes
Cl3 . Cu2 . O1 . 82.95(8) yes
Cl3 . Cu2 . N3 . 93.73(9) yes
O1 . Cu2 . N3 . 176.00(11) yes
Cu1 . Cl1 . Cu2 . 81.52(3) yes
Cu1 3_656 Cl2 . Cu2 . 80.52(3) yes
Cu2 . Cl3 . Cu2 3_656 80.05(4) yes
Cu1 3_656 Cl4 . Cu1 . 79.27(6) yes
Cu2 3_656 O1 . Cu2 . 114.04(15) yes
Cu2 3_656 O1 . Cu1 . 108.355(18) yes
Cu2 . O1 . Cu1 . 107.533(17) yes
Cu2 3_656 O1 . Cu1 3_656 107.533(17) yes
Cu2 . O1 . Cu1 3_656 108.355(18) yes
Cu1 . O1 . Cu1 3_656 111.06(15) yes
Cu1 . N1 . N2 . 121.8(2) yes
Cu1 . N1 . C4 . 131.8(3) yes
N2 . N1 . C4 . 106.2(3) yes
N1 . N2 . C2 . 112.0(3) yes
N1 . N2 . H21 . 123.2 no
C2 . N2 . H21 . 124.7 no
Cu2 . N3 . N4 . 121.6(2) yes
Cu2 . N3 . C7 . 131.5(3) yes
N4 . N3 . C7 . 106.1(3) yes
N3 . N4 . C9 . 111.9(3) yes
N3 . N4 . H41 . 122.6 no
C9 . N4 . H41 . 123.3 no
C2 . C1 . H11 . 110.0 no
C2 . C1 . H13 . 111.5 no
H11 . C1 . H13 . 108.1 no
C2 . C1 . H12 . 110.3 no
H11 . C1 . H12 . 108.0 no
H13 . C1 . H12 . 108.9 no
C1 . C2 . N2 . 121.6(4) yes
C1 . C2 . C3 . 132.6(4) yes
N2 . C2 . C3 . 105.8(3) yes
C2 . C3 . C4 . 107.5(3) yes
C2 . C3 . H31 . 126.2 no
C4 . C3 . H31 . 126.3 no
C3 . C4 . N1 . 108.5(3) yes
C3 . C4 . C5 . 129.4(3) yes
N1 . C4 . C5 . 122.1(3) yes
C4 . C5 . H52 . 111.3 no
C4 . C5 . H51 . 107.1 no
H52 . C5 . H51 . 110.0 no
C4 . C5 . H53 . 109.9 no
H52 . C5 . H53 . 110.7 no
H51 . C5 . H53 . 107.8 no
C7 . C6 . H61 . 112.3 no
C7 . C6 . H63 . 110.4 no
H61 . C6 . H63 . 108.4 no
C7 . C6 . H62 . 109.7 no
H61 . C6 . H62 . 108.7 no
H63 . C6 . H62 . 107.2 no
C6 . C7 . N3 . 121.4(4) yes
C6 . C7 . C8 . 129.5(4) yes
N3 . C7 . C8 . 109.1(4) yes
C7 . C8 . C9 . 107.4(4) yes
C7 . C8 . H81 . 126.9 no
C9 . C8 . H81 . 125.7 no
C8 . C9 . N4 . 105.6(4) yes
C8 . C9 . C10 . 132.9(4) yes
N4 . C9 . C10 . 121.5(5) yes
C9 . C10 . H102 . 109.5 no
C9 . C10 . H101 . 110.2 no
H102 . C10 . H101 . 109.5 no
C9 . C10 . H103 . 109.2 no
H102 . C10 . H103 . 109.3 no
H101 . C10 . H103 . 109.1 no
#------------------------------------------------------------------------------
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
Cl3 Cl4 3.277(2) . 1_545 no
Cl3 Cl4 3.277(2) . 3_646 no
Cl4 N4 3.380(3) . 3_666 no
C5 C5 3.522(8) . 2_766 no
#------------------------------------------------------------------------------
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu1 Cl1 Cu2 Cl2 . . . . 80.46(5) no
Cu1 Cl1 Cu2 Cl3 . . . . -80.51(4) no
Cu1 Cl1 Cu2 O1 . . . . -0.97(6) no
Cu1 Cl1 Cu2 N3 . . . . -176.97(8) no
Cu1 Cl2 Cu2 Cl1 . 3_656 3_656 3_656 -77.45(5) no
Cu1 Cl2 Cu2 Cl3 . 3_656 3_656 . 84.21(4) no
Cu1 Cl2 Cu2 O1 . 3_656 3_656 . 3.85(7) no
Cu1 Cl2 Cu2 N3 . 3_656 3_656 3_656 -178.25(9) no
Cu1 Cl4 Cu1 Cl1 . . 3_656 3_656 99.80(6) no
Cu1 Cl4 Cu1 Cl2 . . 3_656 . -54.7(1) no
Cu1 Cl4 Cu1 Cl4 . . 3_656 3_656 -73.0(1) no
Cu1 Cl4 Cu1 O1 . . 3_656 . 15.62(5) no
Cu1 Cl4 Cu1 N1 . . 3_656 3_656 -163.60(9) no
Cu1 Cl4 Cl4 Cu1 . . 3_656 3_656 86.33(6) no
Cu1 Cl4 Cu1 Cl1 . 3_656 3_656 3_656 58.4(1) no
Cu1 Cl4 Cu1 Cl2 . 3_656 3_656 . -99.10(6) no
Cu1 Cl4 Cu1 Cl4 . 3_656 3_656 . 69.5(1) no
Cu1 Cl4 Cu1 O1 . 3_656 3_656 . -15.56(5) no
Cu1 Cl4 Cu1 N1 . 3_656 3_656 3_656 161.19(9) no
Cu1 Cl4 Cl4 Cu1 . 3_656 . 3_656 -86.33(6) no
Cu1 O1 Cu1 Cl1 . . 3_656 3_656 -119.63(3) no
Cu1 O1 Cu1 Cl2 . . 3_656 . 122.89(3) no
Cu1 O1 Cu1 Cl4 . . 3_656 . -21.24(5) no
Cu1 O1 Cu1 Cl4 . . 3_656 3_656 21.64(6) no
Cu1 O1 Cu2 Cl1 . . . . 1.24(8) no
Cu1 O1 Cu2 Cl2 . . . . -125.16(9) no
Cu1 O1 Cu2 Cl3 . . . . 120.17(8) no
Cu1 O1 Cu2 Cl1 . . 3_656 3_656 121.36(9) no
Cu1 O1 Cu2 Cl2 . . 3_656 3_656 -5.05(8) no
Cu1 O1 Cu2 Cl3 . . 3_656 . -119.71(8) no
Cu1 N1 N2 C2 . . . . -177.4(2) no
Cu1 N1 C4 C3 . . . . 176.9(2) no
Cu1 N1 C4 C5 . . . . -1.9(4) no
Cu2 Cl1 Cu1 Cl2 . . . 3_656 83.08(4) no
Cu2 Cl1 Cu1 Cl4 . . . . -72.02(9) no
Cu2 Cl1 Cu1 Cl4 . . . 3_656 -79.49(6) no
Cu2 Cl1 Cu1 O1 . . . . 0.97(6) no
Cu2 Cl1 Cu1 N1 . . . . -173.56(9) no
Cu2 Cl2 Cu1 Cl1 . . 3_656 3_656 -86.22(4) no
Cu2 Cl2 Cu1 Cl4 . . 3_656 . 65.2(1) no
Cu2 Cl2 Cu1 Cl4 . . 3_656 3_656 77.65(6) no
Cu2 Cl2 Cu1 O1 . . 3_656 . -3.85(6) no
Cu2 Cl2 Cu1 N1 . . 3_656 3_656 172.18(8) no
Cu2 Cl3 Cu2 Cl1 . . 3_656 3_656 81.03(4) no
Cu2 Cl3 Cu2 Cl2 . . 3_656 3_656 -82.16(4) no
Cu2 Cl3 Cu2 O1 . . 3_656 . 0.0000(3) no
Cu2 Cl3 Cu2 N3 . . 3_656 3_656 177.75(9) no
Cu2 O1 Cu1 Cl1 . . . . -1.24(8) no
Cu2 O1 Cu1 Cl2 . . . 3_656 -118.72(9) no
Cu2 O1 Cu1 Cl4 . . . . 140.0(1) no
Cu2 O1 Cu1 Cl4 . . . 3_656 97.15(9) no
Cu2 O1 Cu1 Cl1 . . 3_656 3_656 122.47(9) no
Cu2 O1 Cu1 Cl2 . . 3_656 . 5.00(8) no
Cu2 O1 Cu1 Cl4 . . 3_656 . -139.1(1) no
Cu2 O1 Cu1 Cl4 . . 3_656 3_656 -96.3(1) no
Cu2 O1 Cu2 Cl1 . . 3_656 3_656 -118.93(3) no
Cu2 O1 Cu2 Cl2 . . 3_656 3_656 114.66(3) no
Cu2 O1 Cu2 Cl3 . . 3_656 . 0.0000(4) no
Cu2 N3 N4 C9 . . . . -171.7(3) no
Cu2 N3 C7 C6 . . . . -9.1(6) no
Cu2 N3 C7 C8 . . . . 170.2(3) no
Cl1 Cu1 Cl4 Cl4 . . . 3_656 -11.0(2) no
Cl1 Cu1 Cl4 Cl4 . . 3_656 . 172.8(1) no
Cl1 Cu1 N1 N2 . . . . 121.7(2) no
Cl1 Cu1 N1 C4 . . . . -54.3(3) no
Cl1 Cu2 N3 N4 . . . . 110.0(3) no
Cl1 Cu2 N3 C7 . . . . -58.5(3) no
Cl2 Cu1 Cl4 Cl4 . 3_656 . 3_656 18.4(2) no
Cl2 Cu1 Cl4 Cl4 . 3_656 3_656 . -168.5(1) no
Cl2 Cu1 N1 N2 . 3_656 3_656 3_656 -119.8(2) no
Cl2 Cu1 N1 C4 . 3_656 3_656 3_656 64.2(3) no
Cl2 Cu2 N3 N4 . . . . -123.1(3) no
Cl2 Cu2 N3 C7 . . . . 68.4(3) no
Cl3 Cu2 N3 N4 . . . . -8.4(3) no
Cl3 Cu2 N3 C7 . . . . -176.9(3) no
Cl3 Cu2 N3 N4 . 3_656 3_656 3_656 -8.4(3) no
Cl3 Cu2 N3 C7 . 3_656 3_656 3_656 -176.9(3) no
Cl4 Cu1 Cl4 Cu1 . . 3_656 3_656 -73.0(1) no
Cl4 Cu1 N1 N2 . . . . -18.8(2) no
Cl4 Cu1 N1 C4 . . . . 165.3(3) no
Cl4 Cu1 Cl4 Cu1 . 3_656 3_656 . 69.5(1) no
Cl4 Cu1 N1 N2 . 3_656 3_656 3_656 23.7(2) no
Cl4 Cu1 N1 C4 . 3_656 3_656 3_656 -152.2(3) no
Cl4 Cl4 Cu1 O1 . 3_656 . . 88.6(1) no
Cl4 Cl4 Cu1 N1 . 3_656 . . -90.6(1) no
Cl4 Cl4 Cu1 O1 . 3_656 3_656 . -85.0(1) no
Cl4 Cl4 Cu1 N1 . 3_656 3_656 3_656 91.7(1) no
N1 N2 C2 C1 . . . . 179.4(3) no
N1 N2 C2 C3 . . . . 0.3(4) no
N1 C4 C3 C2 . . . . -0.3(4) no
N2 N1 C4 C3 . . . . 0.5(3) no
N2 N1 C4 C5 . . . . -178.3(3) no
N2 C2 C3 C4 . . . . 0.0(4) no
N3 N4 C9 C8 . . . . 0.6(5) no
N3 N4 C9 C10 . . . . -177.3(4) no
N3 C7 C8 C9 . . . . -0.1(5) no
N4 N3 C7 C6 . . . . -178.9(4) no
N4 N3 C7 C8 . . . . 0.4(4) no
N4 C9 C8 C7 . . . . -0.3(5) no
C1 C2 C3 C4 . . . . -179.0(4) no
C2 N2 N1 C4 . . . . -0.5(4) no
C2 C3 C4 C5 . . . . 178.3(3) no
C6 C7 C8 C9 . . . . 179.2(4) no
C7 N3 N4 C9 . . . . -0.7(4) no
C7 C8 C9 C10 . . . . 177.3(6) no
#------------------------------------------------------------------------------
_iucr_refine_instruction_details_constraints
;
#
# Punched on 02/09/13 at 17:47:12
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE N ( 2,X'S) H ( 21,X'S)
RIDE N ( 4,X'S) H ( 41,X'S)
RIDE C ( 1,X'S) H ( 11,X'S) H ( 13,X'S) H ( 12,X'S)
RIDE C ( 3,X'S) H ( 31,X'S)
RIDE C ( 5,X'S) H ( 52,X'S) H ( 51,X'S) H ( 53,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 63,X'S) H ( 62,X'S)
RIDE C ( 8,X'S) H ( 81,X'S)
RIDE C ( 10,X'S) H ( 102,X'S) H ( 101,X'S) H ( 103,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
#
# Punched on 02/09/13 at 17:47:12
#
#LIST 16
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;
# Manually omitted reflections
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
-1 0 3 x .
-1 0 5 x .
-2 0 2 x .
0 0 4 x .
#===END