data_global
_publ_contact_author_name
;
Anthony Other
;
_publ_contact_author_email 'paul.carr@anu.edu.au'
_publ_contact_author_phone
;
+44 1865 000000
;
_publ_contact_author_fax
;
+44 1865 000000
;
_publ_contact_author_id_iucr ?
_publ_contact_author_address
;
Chemical Crystallography Laboratory,
Department of Chemistry,
University of Nowhere,
Nowhere, NO1 4T, UK.
;
_publ_contact_letter
;
Please consider this CIF submission for
publication as a Short Format Paper in Acta
Crystallographica E.
;
_publ_requested_journal
;
Section E
;
_publ_requested_category 'EO'
_publ_requested_coeditor_name
;
Prof William Clegg
;
loop_
_publ_author_name
_publ_author_address
_publ_author_email
_publ_author_footnote
'Carr, Paul D.'
;
Research School of Chemistry,
Australian National University,
Canberra,
Act 2601,
Australia
;
. .
'Vafazadeh, Rasoul'
;
Department of Chemistry,
Yazd Univeristy,
Safayieh,
Yazd,
Iran
;
. .
'Shahpoori, Behnoosh'
;
Department of Chemistry,
Yazd Univeristy,
Safayieh,
Yazd,
Iran
;
. .
_publ_section_title
;
Structure report for sample SPN (RAS15_PC05X)
;
_publ_section_title_footnote .
_publ_section_synopsis .
_publ_section_abstract
;
The expected structure (C~26~H~50~N~4~Ni~3~O~14~) was not observed in the
crystal, instead a molecule of C~14~H~30~N~4~NiO~4~ was present. A search of
the Cambridge Structural Database did not reveal an existing deposited
structure for this compound.
;
_publ_section_keywords
;
crystal structure
;
loop_
_publ_body_element
_publ_body_title
_publ_body_contents
section
;
Introduction
;
;
;
section
;
Experimental
;
;
;
subsection
;
Synthesis and crystallization
;
;
;
subsection
;
Refinement
;
;
Crystal data, data collection and structure refinement details are summarized in
Table 1. In the absence of significant anomalous scattering, Friedel pairs
were merged.
The absolute configuration was arbitrarily assigned.
Changes in illuminated volume were kept to a minimum, and were taken into
account (G\"orbitz, 1999) by the multi-scan inter-frame scaling
(DENZO/SCALEPACK, Otwinowski & Minor, 1997).
G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098.
The H atoms were all located in a difference map, but those attached to carbon
atoms were repositioned geometrically. The H atoms were initially refined with
soft restraints on the bond lengths and angles to regularise their geometry
(C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86
O---H = 0.82 \%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
(Cooper et al., 2010).
Cooper, R. I., Thompson, A. L. & Watkin, D. J. (2010). J. Appl. Cryst. 43,
1100-1107.
;
section
;
Results and discussion
;
;
;
_publ_section_comment ?
_publ_section_exptl_prep
;
;
_publ_section_exptl_refinement
;
;
_publ_section_acknowledgements
;
(type here to add)
;
_publ_section_references
;
Altomare, A., Cascarano, G., Giacovazzo, C., 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--?.
Agilent Technologies, (2013). Yarnton, England.
Spek, A. L. (2009). Acta Cryst. D65, 148--155.
Watkin, D. J., Prout, C. K. & Pearce, L. J. (1996). CAMERON, Chemical
Crystallography Laboratory, Oxford, UK.
;
_publ_section_related_literature
;
;
_publ_section_figure_captions
;
Fig. 1. The title compound with displacement ellipsoids drawn at the 30%
probability level. H atoms are shown as spheres of arbitary radius.
;
_journal_coden_ASTM ?
_journal_coden_Cambridge ?
_journal_coeditor_address ?
_journal_coeditor_code ?
_journal_coeditor_email ?
_journal_coeditor_fax ?
_journal_coeditor_name ?
_journal_coeditor_notes ?
_journal_coeditor_phone ?
_journal_data_validation_number ?
_journal_date_accepted ?
_journal_date_from_coeditor ?
_journal_date_to_coeditor ?
_journal_date_printers_final ?
_journal_date_printers_first ?
_journal_date_proofs_in ?
_journal_date_proofs_out ?
_journal_date_recd_copyright ?
_journal_date_recd_electronic ?
_journal_date_recd_hard_copy ?
_journal_issue ?
_journal_language ?
_journal_name_full ?
_journal_page_first ?
_journal_page_last ?
_journal_paper_category ?
_journal_paper_doi ?
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
_journal_techeditor_address ?
_journal_techeditor_code ?
_journal_techeditor_email ?
_journal_techeditor_fax ?
_journal_techeditor_name ?
_journal_techeditor_notes ?
_journal_techeditor_phone ?
_journal_volume ?
_journal_year ?
_iucr_compatibility_tag ?
# publcif _publ_body_element loop start
# publcif _publ_body_element loop end
_audit_update_record
;
2015-05-21 # Formatted by publCIF
;
_publcif_datablock.id '{b04a2223-6753-451d-8290-1793c697e365}'
_audit_creation_date "2015-05-20"
_audit_creation_method CRYSTALS_ver_14.43
_oxford_structure_analysis_title 'C:\Users\PaulCarr\Desktop\ras15_ At 12: 4 on'
_chemical_name_systematic ?
_chemical_melting_point ?
#looking for refcif
# Check this file using the IUCr facility at:
# http://checkcif.iucr.org/
# The content below is held in the file 'script/refcif.dat'. This is a text
# file which you may edit to reflect local conditions.
# Items which need looking at are represented by a '?'.
# Items for which there are choices are prefixed with 'choose from'.
# choose from: FI FM FO CI CM CO AD
# The loop structure below should contain the names and addresses of all
# authors, in the required order of publication. Repeat as necessary.
# Hand-made tables can be put in the cif. The number of columns
# is set in the loop header.
# The contants of each column can either be a piece of text
# without any spaces (eg a number) or other text enclosed in " "
# Remove the leading # in the following example
#geom_extra_table_head_A
#;
#Table 2.
#Molecular parameters deviating most from MOGUL averages
#;
#
#loop_
#_geom_extra_tableA_col_1
#_geom_extra_tableA_col_2
#_geom_extra_tableA_col_3
#_geom_extra_tableA_col_4
#
#Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d"
#N5-C6-C4 129 124 "7 (\%)"
#C3-O10-C2 105 109 "2 (\%)"
#C6-O7 1.25 1.22 ".02 (\%A)"
#
data_1
_diffrn_radiation_source MoKa
#Added by publCIF
_publcif_datablock.id '{a0ec8999-d4fe-41b0-a8f4-482eeb63f3b1}'
_exptl_special_details
;
The crystal was
placed in the cold stream of an Oxford
Cryosystems open-flow nitrogen cryostat (Cosier &
Glazer, 1986) with a nominal stability of 0.1K.
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107.
;
_refine_special_details
?
#---------------------------------------------------------------
# _oxford_ data items, April 2010:
# There is some uncertainty about the correct way of forming local data
# names, e.g.
# _atom_site_special_shape_oxford
# or
# _oxford_atom_site_special_shape
# see:
# http://www.iucr.org/resources/cif/spec/version1.1/semantics#namespace
# A reserved prefix, e.g. foo, must be used in the following way
# " If the data file contains items defined in a DDL1 dictionary, the
# local data names assigned under the reserved prefix must contain it as
# their first component, e.g. _foo_atom_site_my_item. "
# However, this seems to say the opposite:
# http://www.iucr.org/__data/iucr/cif/standard/cifstd8.html
# According to advice from the IUCr, CRYSTALS is correct
#---------------------------------------------------------------
# End of 'script/refcif.dat'
#end of refcif
_cell_length_a 10.0738(5)
_cell_length_b 8.3205(3)
_cell_length_c 11.1221(6)
_cell_angle_alpha 90
_cell_angle_beta 103.659(5)
_cell_angle_gamma 90
_cell_volume 905.88(8)
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/c 1 '
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x,y,z'
'-x,-y,-z'
'-x,y+1/2,-z+1/2'
'x,-y+1/2,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'
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'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763
2.3800 66.3421 1.0341 '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 = C14 H32 N4 Ni1 O4
# Dc = 1.39 Fooo = 404.00 Mu = 10.95 M = 189.57
# Found Formula = C14 H30 N4 Ni1 O4
# Dc = 1.38 FOOO = 404.00 Mu = 10.95 M = 188.56
_chemical_formula_sum 'C14 H30 N4 Ni1 O4'
_chemical_formula_moiety 'C14 H30 N4 Ni1 O4'
_chemical_compound_source ?
_chemical_formula_weight 377.13
_cell_measurement_reflns_used 3939
_cell_measurement_theta_min 3
_cell_measurement_theta_max 29
_cell_measurement_temperature 150
_exptl_crystal_description 'plate'
_exptl_crystal_colour 'mauve'
_exptl_crystal_size_min 0.095
_exptl_crystal_size_mid 0.191
_exptl_crystal_size_max 0.271
_exptl_crystal_density_diffrn 1.383
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
# Non-dispersive F(000):
_exptl_crystal_F_000 404
_exptl_absorpt_coefficient_mu 1.095
# Sheldrick geometric approximatio 0.81 0.90
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies, (2013), Yarnton, England
;
_exptl_absorpt_correction_T_min 0.64
_exptl_absorpt_correction_T_max 0.90
_diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device 'Area'
_diffrn_radiation_monochromator 'graphite'
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_measurement_method \w
# If a reference occurs more than once, delete the author
# and date from subsequent references.
_computing_data_collection 'Xcalibur, (Agilent Technologies, (2013),'
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies, (2013), Yarnton, England
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies, (2013), Yarnton, England
;
_computing_structure_solution 'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material 'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics 'PLATON (Spek, 2009)'
_diffrn_standards_interval_time .
_diffrn_standards_interval_count .
_diffrn_standards_number 0
_diffrn_standards_decay_% ?
_diffrn_ambient_temperature 150
_diffrn_reflns_number 10433
_reflns_number_total 2280
_diffrn_reflns_av_R_equivalents 0.044
# Number of reflections without Friedels Law is 0
# Number of reflections with Friedels Law is 2280
# Theoretical number of reflections is about 5081
_diffrn_reflns_theta_min 2.080
_diffrn_reflns_theta_max 29.570
_diffrn_measured_fraction_theta_max 0.897
_diffrn_reflns_theta_full 25.135
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -11
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -15
_diffrn_reflns_limit_l_max 13
_reflns_limit_h_min -13
_reflns_limit_h_max 13
_reflns_limit_k_min 0
_reflns_limit_k_max 11
_reflns_limit_l_min 0
_reflns_limit_l_max 15
_oxford_diffrn_Wilson_B_factor 1.50
_oxford_diffrn_Wilson_scale 0.07
_atom_sites_solution_primary direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens difmap
_refine_diff_density_min -0.63
_refine_diff_density_max 1.06
# 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 2270
_refine_ls_number_restraints 0
_refine_ls_number_parameters 106
_oxford_refine_ls_R_factor_ref 0.0558
_refine_ls_wR_factor_ref 0.0975
_refine_ls_goodness_of_fit_ref 3.5922
_refine_ls_shift/su_max 0.0118546
_refine_ls_shift/su_mean 0.0029550
# The values computed with all filters except I/sigma
_oxford_reflns_number_all 2270
_refine_ls_R_factor_all 0.0558
_refine_ls_wR_factor_all 0.0975
# The values computed with a 2 sigma cutoff - a la SHELX
_reflns_threshold_expression I>2.0\s(I)
_reflns_number_gt 1868
_refine_ls_R_factor_gt 0.0432
_refine_ls_wR_factor_gt 0.0845
# 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
# WARNING. The IUCr will not accept Unit Weights
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
;
Method= Quasi-Unit weights
W = 1.0 or 1./2F
;
# Insert your own references if required - in alphabetical order
# 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
O1 O 0.8155(2) 0.5341(2) 0.36357(17) 0.0249 1.0000 Uani . . . . . .
O2 O 0.8659(2) 0.7445(3) 0.25669(19) 0.0306 1.0000 Uani . . . . . .
N1 N 1.0028(2) 0.7470(3) 0.5417(2) 0.0238 1.0000 Uani . . . . . .
C1 C 1.1361(3) 0.8286(3) 0.5670(3) 0.0283 1.0000 Uani . . . . . .
C2 C 1.1976(3) 0.8280(3) 0.4544(3) 0.0298 1.0000 Uani . . . . . .
C3 C 1.2380(3) 0.6625(3) 0.4165(3) 0.0270 1.0000 Uani . . . . . .
C4 C 0.7856(3) 0.6384(3) 0.2785(2) 0.0227 1.0000 Uani . . . . . .
C5 C 0.6421(3) 0.6324(3) 0.1968(3) 0.0282 1.0000 Uani . . . . . .
C6 C 0.6134(3) 0.7248(4) 0.0884(3) 0.0391 1.0000 Uani . . . . . .
C7 C 0.5454(3) 0.5305(5) 0.2327(4) 0.0478 1.0000 Uani . . . . . .
Ni1 Ni 1.0000 0.5000 0.5000 0.0184 1.0000 Uani S . . . . .
N2 N 1.1174(2) 0.5584(3) 0.3728(2) 0.0218 1.0000 Uani . . . . . .
H1 H 1.1295 0.9381 0.5941 0.0343 1.0000 Uiso R . . . . .
H2 H 1.2972 0.6089 0.4883 0.0324 1.0000 Uiso R . . . . .
H3 H 1.1987 0.7714 0.6328 0.0336 1.0000 Uiso R . . . . .
H4 H 0.5250 0.6999 0.0332 0.0587 1.0000 Uiso R . . . . .
H5 H 0.9456 0.7940 0.4782 0.0361 1.0000 Uiso R . . . . .
H6 H 1.2888 0.6736 0.3512 0.0334 1.0000 Uiso R . . . . .
H7 H 0.4587 0.5205 0.1796 0.0568 1.0000 Uiso R . . . . .
H8 H 1.1314 0.8752 0.3855 0.0362 1.0000 Uiso R . . . . .
H9 H 1.1422 0.4703 0.3402 0.0328 1.0000 Uiso R . . . . .
H11 H 1.2819 0.8942 0.4749 0.0362 1.0000 Uiso R . . . . .
H12 H 0.9659 0.7598 0.6078 0.0354 1.0000 Uiso R . . . . .
H13 H 1.0619 0.6056 0.3092 0.0333 1.0000 Uiso R . . . . .
H14 H 0.6856 0.7226 0.0441 0.0598 1.0000 Uiso R . . . . .
H15 H 0.5665 0.4803 0.3082 0.0583 1.0000 Uiso R . . . . .
H17 H 0.6094 0.8344 0.1121 0.0606 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
O1 0.0279(10) 0.0220(9) 0.0238(9) 0.0036(7) 0.0037(7) -0.0016(8)
O2 0.0304(11) 0.0283(10) 0.0322(11) 0.0120(9) 0.0055(9) 0.0001(9)
N1 0.0315(12) 0.0154(10) 0.0242(11) -0.0003(8) 0.0058(9) 0.0010(9)
C1 0.0358(16) 0.0173(12) 0.0307(14) -0.0019(11) 0.0054(12) -0.0029(11)
C2 0.0359(16) 0.0218(13) 0.0316(15) 0.0028(11) 0.0077(12) -0.0071(12)
C3 0.0286(14) 0.0270(14) 0.0265(14) 0.0031(11) 0.0090(11) -0.0037(11)
C4 0.0269(13) 0.0199(12) 0.0221(12) -0.0008(10) 0.0073(10) 0.0024(10)
C5 0.0282(14) 0.0249(13) 0.0303(15) 0.0002(11) 0.0048(11) 0.0051(11)
C6 0.0360(17) 0.0364(17) 0.0407(18) 0.0020(14) 0.0004(14) 0.0055(14)
C7 0.0258(15) 0.062(3) 0.051(2) 0.0150(19) -0.0006(14) -0.0074(16)
Ni1 0.0242(2) 0.0127(2) 0.0188(2) 0.00072(17) 0.00569(16) -0.00039(18)
N2 0.0262(11) 0.0188(10) 0.0207(10) 0.0016(8) 0.0059(8) 0.0008(9)
_refine_ls_extinction_method
'None'
_oxford_refine_ls_scale 3.82(5)
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
O1 . C4 . 1.267(3) yes
O1 . Ni1 . 2.1225(19) yes
O2 . C4 . 1.260(3) yes
N1 . C1 . 1.472(4) yes
N1 . Ni1 . 2.105(2) yes
N1 . H5 . 0.889 no
N1 . H12 . 0.905 no
C1 . C2 . 1.523(4) yes
C1 . H1 . 0.966 no
C1 . H3 . 0.971 no
C2 . C3 . 1.524(4) yes
C2 . H8 . 0.973 no
C2 . H11 . 0.992 no
C3 . N2 . 1.478(3) yes
C3 . H2 . 0.983 no
C3 . H6 . 0.986 no
C4 . C5 . 1.515(4) yes
C5 . C6 . 1.401(4) yes
C5 . C7 . 1.419(4) yes
C6 . H4 . 0.977 no
C6 . H14 . 0.970 no
C6 . H17 . 0.953 no
C7 . H7 . 0.935 no
C7 . H15 . 0.917 no
Ni1 . N2 2_766 2.104(2) yes
Ni1 . N2 . 2.104(2) yes
N2 . H9 . 0.880 no
N2 . H13 . 0.883 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
C4 . O1 . Ni1 . 129.76(18) yes
C1 . N1 . Ni1 . 117.17(17) yes
C1 . N1 . H5 . 109.8 no
Ni1 . N1 . H5 . 106.4 no
C1 . N1 . H12 . 108.7 no
Ni1 . N1 . H12 . 107.9 no
H5 . N1 . H12 . 106.2 no
N1 . C1 . C2 . 111.8(2) yes
N1 . C1 . H1 . 111.6 no
C2 . C1 . H1 . 109.3 no
N1 . C1 . H3 . 108.6 no
C2 . C1 . H3 . 107.4 no
H1 . C1 . H3 . 107.9 no
C1 . C2 . C3 . 114.7(2) yes
C1 . C2 . H8 . 108.0 no
C3 . C2 . H8 . 109.0 no
C1 . C2 . H11 . 107.6 no
C3 . C2 . H11 . 107.2 no
H8 . C2 . H11 . 110.3 no
C2 . C3 . N2 . 111.6(2) yes
C2 . C3 . H2 . 109.6 no
N2 . C3 . H2 . 107.2 no
C2 . C3 . H6 . 109.7 no
N2 . C3 . H6 . 110.0 no
H2 . C3 . H6 . 108.7 no
O1 . C4 . O2 . 125.0(3) yes
O1 . C4 . C5 . 116.8(2) yes
O2 . C4 . C5 . 118.2(2) yes
C4 . C5 . C6 . 118.2(3) yes
C4 . C5 . C7 . 118.1(3) yes
C6 . C5 . C7 . 123.7(3) yes
C5 . C6 . H4 . 113.4 no
C5 . C6 . H14 . 113.5 no
H4 . C6 . H14 . 111.0 no
C5 . C6 . H17 . 107.5 no
H4 . C6 . H17 . 106.6 no
H14 . C6 . H17 . 104.1 no
C5 . C7 . H7 . 118.4 no
C5 . C7 . H15 . 120.3 no
H7 . C7 . H15 . 121.2 no
O1 . Ni1 . O1 2_766 179.995 yes
O1 . Ni1 . N1 . 89.47(8) yes
O1 2_766 Ni1 . N1 . 90.53(8) yes
O1 . Ni1 . N1 2_766 90.53(8) yes
O1 2_766 Ni1 . N1 2_766 89.47(8) yes
N1 . Ni1 . N1 2_766 179.995 yes
O1 . Ni1 . N2 2_766 88.59(8) yes
O1 2_766 Ni1 . N2 2_766 91.41(8) yes
N1 . Ni1 . N2 2_766 93.31(9) yes
N1 2_766 Ni1 . N2 2_766 86.69(9) yes
O1 . Ni1 . N2 . 91.41(8) yes
O1 2_766 Ni1 . N2 . 88.59(8) yes
N1 . Ni1 . N2 . 86.69(9) yes
N1 2_766 Ni1 . N2 . 93.31(9) yes
N2 2_766 Ni1 . N2 . 179.995 yes
C3 . N2 . Ni1 . 117.61(17) yes
C3 . N2 . H9 . 109.4 no
Ni1 . N2 . H9 . 110.1 no
C3 . N2 . H13 . 108.6 no
Ni1 . N2 . H13 . 107.0 no
H9 . N2 . H13 . 103.2 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
N1 . H5 . O2 . 136.43(7) 0.889 2.440 3.144(4) yes
N2 . H9 . O2 3_745 161.85(8) 0.880 2.157 3.007(4) yes
N1 . H12 . O2 4_565 171.44(8) 0.905 2.132 3.030(4) yes
N2 . H13 . O2 . 142.10(8) 0.883 2.243 2.989(4) yes
_iucr_refine_instructions_details_constraints
;
#
# Punched on 20/05/15 at 15:51:26
#
#LIST 12
BLOCK SCALE X'S, U'S
RIDE N ( 1,X'S) H ( 5,X'S) H ( 12,X'S)
RIDE C ( 1,X'S) H ( 1,X'S) H ( 3,X'S)
RIDE C ( 2,X'S) H ( 8,X'S) H ( 11,X'S)
RIDE C ( 3,X'S) H ( 2,X'S) H ( 6,X'S)
RIDE C ( 6,X'S) H ( 4,X'S) H ( 14,X'S) H ( 17,X'S)
RIDE C ( 7,X'S) H ( 7,X'S) H ( 15,X'S)
RIDE N ( 2,X'S) H ( 9,X'S) H ( 13,X'S)
END
;
_iucr_refine_instructions_details_restraints
;
#
# Punched on 20/05/15 at 15:51:26
#
#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 0 x .
1 0 2 x .
-10 3 11 x .
9 1 8 x .
-10 3 12 x .
-13 1 6 x .
-6 1 12 x .
11 5 3 x .
2 2 13 x .
-13 2 3 x .
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
'{b04a2223-6753-451d-8290-1793c697e365}' ? ? ?
'{a0ec8999-d4fe-41b0-a8f4-482eeb63f3b1}' y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item
?
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
"{b04a2223-6753-451d-8290-1793c697e365}" "_publcif_info_datablock.publ_exptl"
"{a0ec8999-d4fe-41b0-a8f4-482eeb63f3b1}" "_geom_bond_atom_site_label_1"
"{a0ec8999-d4fe-41b0-a8f4-482eeb63f3b1}" "_geom_hbond_atom_site_label_D"
loop_
_publcif_info_cif.paper_type
?