data_ras1506SN _audit_creation_date "15-05-21" _audit_creation_method CRYSTALS_ver_14.40 _audit_update_record ; 2015-05-21 - Report on C12 H30 N4 Ni O6 by Anthony C. Willis for Rasoul Vafazadeh and Behnoosh Shahpoori 2015-05-21 - passes checkcif tests with minor warnings ; _oxford_structure_analysis_title 'Z:\ras1506SN\Tony_ras1506aSN\ras At 10: 2 on' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 24.4016(10) _cell_length_b 6.9977(3) _cell_length_c 10.7021(6) _cell_angle_alpha 90 _cell_angle_beta 93.316(4) _cell_angle_gamma 90 _cell_volume 1824.38(15) _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' 'x+1/2,y+1/2,z' '-x+1/2,-y+1/2,-z' 'x,-y,z+1/2' '-x,y,-z+1/2' 'x+1/2,-y+1/2,z+1/2' '-x+1/2,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 0.0181 0.0091 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 0.0311 0.0180 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 -3.0029 0.5091 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 0.0492 0.0322 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 4 # Given Formula = C10 H20 N2 Ni1 O5 # Dc = 1.12 Fooo = 824.00 Mu = 16.53 M = 153.49 # Found Formula = C12 H30 N4 Ni1 O6 # Dc = 1.40 FOOO = 824.00 Mu = 18.36 M = 192.55 _chemical_formula_sum 'C12 H30 N4 Ni O6' _chemical_formula_moiety 'C4 H20 N4 Ni O2 2+, (C4 H5 O2 -)2' _chemical_compound_source ' Yazd University ' _chemical_formula_weight 385.10 _cell_measurement_reflns_used 5267 _cell_measurement_theta_min 7 _cell_measurement_theta_max 72 _cell_measurement_temperature 150 _exptl_crystal_description 'plate' _exptl_crystal_colour 'violet' _exptl_crystal_size_min 0.028 _exptl_crystal_size_mid 0.360 _exptl_crystal_size_max 0.516 _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.836 # Sheldrick geometric approximatio 0.52 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_T_max 0.95 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, EosS2' _diffrn_radiation_source 'Supernova (Cu) X-ray Source' _diffrn_measurement_device 'Area' _diffrn_radiation_monochromator 'mirror' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET) (compiled Feb 9 2015,16:26:32) ; _computing_cell_refinement 'CrysAlisPro (Agilent Technologies, 2015)' _computing_data_reduction 'CrysAlisPro (Agilent Technologies, 2015)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' ##??? _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'PLATON (Spek, 2008)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 9955 _reflns_number_total 1803 _diffrn_reflns_av_R_equivalents 0.036 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 1803 # Theoretical number of reflections is about 3622 _diffrn_reflns_theta_min 3.629 _diffrn_reflns_theta_max 72.575 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 72.575 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -29 _reflns_limit_h_max 30 _reflns_limit_k_min 0 _reflns_limit_k_max 8 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 1.62 _oxford_diffrn_Wilson_scale 0.22 _atom_sites_solution_primary Other #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.50 _refine_diff_density_max 0.46 # 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 1803 _refine_ls_number_restraints 46 _refine_ls_number_parameters 156 _oxford_refine_ls_R_factor_ref 0.0550 _refine_ls_wR_factor_ref 0.1591 _refine_ls_goodness_of_fit_ref 1.1489 _refine_ls_shift/su_max 0.0031890 _refine_ls_shift/su_mean 0.0003949 # The values computed with all filters except I/sigma _oxford_reflns_number_all 1803 _refine_ls_R_factor_all 0.0550 _refine_ls_wR_factor_all 0.1591 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1710 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_gt 0.1586 # 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 mixed #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^) + ( 0.05P)^2^ +15.78P] ,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. 2601, 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 ' Anthony.Willis@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 [Ni(C~2~H~8~N~2~)~2~(H~2~O)~2~](C~4~H~5~O~2~)~2~ --- ras1506SN ; # 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 ' Behnoosh Shahpoori ' ; 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. 2601, Australia ; #============================================================================== # 4. TEXT _publ_section_abstract #Text of the abstract ; The crystal structure of [Ni(C~2~H~8~N~2~)~2~(H~2~O)~2~](C~4~H~5~O~2~)~2~ is reported. ; _publ_section_comment #Text of the paper ; The crystallographic asymmetric unit consists of one half of a [Ni(C~2~H~8~N~2~)~2~(H~2~O)~2~]^2+^ cation and a (C~4~H~5~O~2~)^-^ anion. The other half of the cation is generated by a crystallographic inversion symmetry operation. ; _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 BS and was recrystallised from dichloromethane/toluene (1/1 V:V). The sample identification was sen. ; _refine_special_details #Text of the paper ; The program PLATON was used to examine the structure and its data, and it suggested a twinning operation which would aid the refinement. Application of this twinning correction within CRYSTALS gave a significant improvement in the agreement factors. The distances to the terminal C atoms of the anion were initially found to be near equal. This suggests that, within the crystallographic lattice, the methyl (---CH~3~) and methylene (\\db CH~2~) groups of C~4~H~5~O~2~^-^ pack randomly at these positions. A model was introduced to emulate the disorder, with C51(methyl) and C61(methylene) for one image and C52(methylene) and C62(methyl) for the other (C51 near-coincident with C52; C61 near-coincident with C62). Distances and angles were restrained to match values obtained for methylacrylates in non-disordered structures, and displacement parameters were restrained to be near-equal for adjacent C sites. The relative occupancies were refined. The H atoms of the cation were all located in a difference electron density map, but were repositioned geometrically. These 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\%A, N---H = 0.87\%A) and with U~iso~(H) in the range 1.2-1.5 times U~eq~ of the parent atom, after which the positions were refined without restraints. The H atoms of the anion were included at calculated positions and ride on the atom site to which they are bonded. The largest peaks in the final difference electron density map are located randomly through the structure. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Palatinus, L. & Chapuis, G. (2007). SUPERFLIP. J. Appl. Cryst., 40, 786-790. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) Spek, A.L. (2008). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; # 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 Ni1 Ni 0.7500 0.7500 0.5000 0.0147 1.0000 Uani S . . . . . O1 O 0.75350(12) 0.4793(4) 0.5969(2) 0.0199 1.0000 Uani . . . . . . O2 O 0.65317(11) 0.2363(4) 0.4015(3) 0.0220 1.0000 Uani . . . . . . O3 O 0.66062(11) 0.2600(4) 0.6097(3) 0.0219 1.0000 Uani . . . . . . N1 N 0.69241(13) 0.8401(5) 0.6244(3) 0.0186 1.0000 Uani . . . . . . N2 N 0.68013(13) 0.6636(5) 0.3908(3) 0.0180 1.0000 Uani . . . . . . C1 C 0.63893(16) 0.7524(6) 0.5868(4) 0.0238 1.0000 Uani . . . . . . C2 C 0.63114(16) 0.7464(6) 0.4451(4) 0.0237 1.0000 Uani . . . . . . C3 C 0.63269(15) 0.2490(5) 0.5067(4) 0.0178 1.0000 Uani D . . . . . C4 C 0.57077(15) 0.2503(7) 0.5097(4) 0.0264 1.0000 Uani D U . . . . C51 C 0.5387(5) 0.256(3) 0.3883(12) 0.0304 0.52(3) Uani D U P . . . C52 C 0.5401(5) 0.205(3) 0.4062(14) 0.0304 0.48(3) Uani D U P . . . C61 C 0.5478(5) 0.243(3) 0.6219(13) 0.0342 0.52(3) Uani D U P . . . C62 C 0.5473(6) 0.300(3) 0.6314(13) 0.0341 0.48(3) Uani D U P . . . H11 H 0.637(2) 0.621(8) 0.619(4) 0.0292 1.0000 Uiso . . . . . . H12 H 0.608(2) 0.823(8) 0.618(4) 0.0293 1.0000 Uiso . . . . . . H21 H 0.6274(19) 0.882(8) 0.413(4) 0.0282 1.0000 Uiso . . . . . . H22 H 0.598(2) 0.669(7) 0.418(4) 0.0281 1.0000 Uiso . . . . . . H511 H 0.5006 0.2560 0.4022 0.0372 0.52 Uiso R . . . . . H512 H 0.5472 0.1463 0.3405 0.0372 0.52 Uiso R . . . . . H513 H 0.5478 0.3679 0.3441 0.0372 0.52 Uiso R . . . . . H521 H 0.5572 0.1730 0.3315 0.0372 0.48 Uiso R . . . . . H522 H 0.5012 0.2058 0.4076 0.0372 0.48 Uiso R . . . . . H611 H 0.5704 0.2376 0.6971 0.0414 0.52 Uiso R . . . . . H612 H 0.5090 0.2437 0.6252 0.0414 0.52 Uiso R . . . . . H621 H 0.5084 0.2960 0.6223 0.0414 0.48 Uiso R . . . . . H622 H 0.5599 0.2101 0.6934 0.0414 0.48 Uiso R . . . . . H623 H 0.5589 0.4243 0.6559 0.0414 0.48 Uiso R . . . . . H811 H 0.7008(19) 0.807(7) 0.710(5) 0.0278 1.0000 Uiso . . . . . . H812 H 0.687(2) 0.968(8) 0.623(4) 0.0281 1.0000 Uiso . . . . . . H821 H 0.682(2) 0.693(7) 0.309(5) 0.0265 1.0000 Uiso . . . . . . H822 H 0.676(2) 0.536(8) 0.393(4) 0.0270 1.0000 Uiso . . . . . . H911 H 0.786(2) 0.404(7) 0.590(4) 0.0304 1.0000 Uiso . . . . . . H912 H 0.725(2) 0.410(8) 0.595(5) 0.0304 1.0000 Uiso . . . . . . 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 Ni1 0.0162(4) 0.0127(4) 0.0151(5) -0.0002(3) 0.0006(3) -0.0002(4) O1 0.0179(13) 0.0165(13) 0.0253(13) 0.0045(11) 0.0010(11) -0.0008(11) O2 0.0224(13) 0.0212(14) 0.0225(14) 0.0006(11) 0.0036(10) 0.0009(12) O3 0.0224(13) 0.0206(14) 0.0226(14) -0.0009(11) 0.0008(10) -0.0016(12) N1 0.0184(16) 0.0172(16) 0.0204(16) -0.0006(13) 0.0035(12) 0.0007(13) N2 0.0177(16) 0.0165(16) 0.0196(16) 0.0009(13) -0.0009(12) -0.0015(13) C1 0.0196(18) 0.020(2) 0.032(2) -0.0004(17) 0.0073(16) 0.0021(17) C2 0.0179(18) 0.021(2) 0.032(2) -0.0013(17) -0.0026(15) 0.0010(17) C3 0.0218(18) 0.0088(16) 0.0227(19) 0.0008(13) 0.0021(14) 0.0002(15) C4 0.0218(18) 0.028(2) 0.029(2) 0.0019(16) 0.0029(15) -0.0010(17) C51 0.023(2) 0.034(6) 0.034(4) 0.014(4) -0.003(2) 0.005(3) C52 0.023(2) 0.034(6) 0.034(4) 0.014(4) -0.003(2) 0.005(3) C61 0.025(2) 0.038(6) 0.040(3) -0.011(4) 0.009(2) 0.007(4) C62 0.025(2) 0.037(6) 0.040(3) -0.012(4) 0.009(2) 0.007(4) _refine_ls_extinction_method 'None' _oxford_refine_ls_scale 2.42(5) loop_ _oxford_twin_element_scale_factors 0.824(4) 0.176(4) 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 Ni1 . O1 4_666 2.159(3) yes Ni1 . N2 4_666 2.099(3) yes Ni1 . N1 4_666 2.088(3) yes Ni1 . O1 . 2.159(3) yes Ni1 . N1 . 2.088(3) yes Ni1 . N2 . 2.099(3) yes O1 . H911 . 0.96(5) no O1 . H912 . 0.84(6) no O2 . C3 . 1.261(5) yes O3 . C3 . 1.264(5) yes N1 . C1 . 1.476(5) yes N1 . H811 . 0.95(5) no N1 . H812 . 0.91(5) no N2 . C2 . 1.477(5) yes N2 . H821 . 0.91(5) no N2 . H822 . 0.90(5) no C1 . C2 . 1.518(6) yes C1 . H11 . 0.98(5) no C1 . H12 . 0.98(5) no C2 . H21 . 1.01(5) no C2 . H22 . 1.00(5) no C3 . C4 . 1.513(5) yes C4 . C51 . 1.478(13) yes C4 . C52 . 1.338(14) yes C4 . C61 . 1.355(14) yes C4 . C62 . 1.493(14) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no C51 . H513 . 0.950 no C51 . H521 . 0.969 no C52 . H521 . 0.950 no C52 . H522 . 0.950 no C61 . H611 . 0.950 no C61 . H612 . 0.950 no C62 . H621 . 0.950 no C62 . H622 . 0.950 no C62 . H623 . 0.950 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 O1 4_666 Ni1 . N2 4_666 91.32(12) yes O1 4_666 Ni1 . N1 4_666 88.17(12) yes N2 4_666 Ni1 . N1 4_666 83.51(13) yes O1 4_666 Ni1 . O1 . 180.0 yes N2 4_666 Ni1 . O1 . 88.68(12) yes N1 4_666 Ni1 . O1 . 91.83(12) yes O1 4_666 Ni1 . N1 . 91.83(12) yes N2 4_666 Ni1 . N1 . 96.49(13) yes N1 4_666 Ni1 . N1 . 180.0 yes O1 . Ni1 . N1 . 88.17(12) yes O1 4_666 Ni1 . N2 . 88.68(12) yes N2 4_666 Ni1 . N2 . 180.0 yes N1 4_666 Ni1 . N2 . 96.49(13) yes O1 . Ni1 . N2 . 91.32(12) yes N1 . Ni1 . N2 . 83.51(13) yes Ni1 . O1 . H911 . 117(3) no Ni1 . O1 . H912 . 119(3) no H911 . O1 . H912 . 111(4) no Ni1 . N1 . C1 . 108.5(2) yes Ni1 . N1 . H811 . 115(3) no C1 . N1 . H811 . 107(3) no Ni1 . N1 . H812 . 113(3) no C1 . N1 . H812 . 107(3) no H811 . N1 . H812 . 106(4) no Ni1 . N2 . C2 . 108.5(2) yes Ni1 . N2 . H821 . 114(3) no C2 . N2 . H821 . 112(3) no Ni1 . N2 . H822 . 111(3) no C2 . N2 . H822 . 106(3) no H821 . N2 . H822 . 105(4) no N1 . C1 . C2 . 110.0(3) yes N1 . C1 . H11 . 110(3) no C2 . C1 . H11 . 109(3) no N1 . C1 . H12 . 113(3) no C2 . C1 . H12 . 107(3) no H11 . C1 . H12 . 107(4) no C1 . C2 . N2 . 110.3(3) yes C1 . C2 . H21 . 109(3) no N2 . C2 . H21 . 107(3) no C1 . C2 . H22 . 111(3) no N2 . C2 . H22 . 110(3) no H21 . C2 . H22 . 110(4) no O3 . C3 . O2 . 124.1(3) yes O3 . C3 . C4 . 118.0(3) yes O2 . C3 . C4 . 117.9(3) yes C3 . C4 . C51 . 117.4(5) yes C3 . C4 . C52 . 119.4(6) yes C3 . C4 . C61 . 118.9(6) yes C51 . C4 . C61 . 123.7(6) yes C3 . C4 . C62 . 117.0(6) yes C52 . C4 . C62 . 123.5(6) yes C4 . C51 . H511 . 109.6 no C4 . C51 . H512 . 109.4 no H511 . C51 . H512 . 109.5 no C4 . C51 . H513 . 109.4 no H511 . C51 . H513 . 109.5 no H512 . C51 . H513 . 109.5 no C4 . C52 . H521 . 120.2 no C4 . C52 . H522 . 119.8 no H521 . C52 . H522 . 120.0 no C4 . C61 . H611 . 120.2 no C4 . C61 . H612 . 119.8 no H611 . C61 . H612 . 120.0 no C4 . C61 . H621 . 115.1 no C4 . C62 . H621 . 109.7 no C4 . C62 . H622 . 109.4 no H621 . C62 . H622 . 109.5 no C4 . C62 . H623 . 109.3 no H621 . C62 . H623 . 109.5 no H622 . C62 . H623 . 109.5 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 . H811 . O1 8_656 135(4) 0.95(5) 2.59(5) 3.337(4) yes N1 . H811 . O2 5_565 139(4) 0.95(5) 2.44(5) 3.214(4) yes N1 . H812 . O3 1_565 170(4) 0.91(5) 2.15(5) 3.041(4) yes N2 . H821 . O3 5_564 164(4) 0.91(5) 2.19(5) 3.066(4) yes N2 . H822 . O2 . 171(4) 0.90(5) 2.17(5) 3.066(4) yes O1 . H911 . O2 4_656 172(4) 0.96(5) 1.78(5) 2.731(4) yes O1 . H912 . O3 . 173(5) 0.84(6) 1.91(6) 2.747(4) yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Ni1 N1 C1 -77.0(3) . . . . no N2 Ni1 N1 C1 14.6(3) . . . . no O1 Ni1 N1 C1 103.0(3) 4_666 . . . no N2 Ni1 N1 C1 -165.4(3) 4_666 . . . no O1 Ni1 N2 C2 99.6(3) . . . . no N1 Ni1 N2 C2 11.6(3) . . . . no O1 Ni1 N2 C2 -80.4(3) 4_666 . . . no N1 Ni1 N2 C2 -168.4(3) 4_666 . . . no Ni1 N1 C1 C2 -37.9(4) . . . . no Ni1 N2 C2 C1 -35.4(4) . . . . no N1 C1 C2 N2 49.7(4) . . . . no O2 C3 C4 C51 -6.0(11) . . . . no O2 C3 C4 C61 173.0(11) . . . . no O3 C3 C4 C51 174.3(10) . . . . no O3 C3 C4 C61 -6.8(12) . . . . 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 O1 O3 2.747(4) . . no O1 N1 2.955(4) . . no O1 N2 3.046(4) . . no O1 C1 3.383(5) . . no O1 N1 3.051(4) . 4_666 no O1 N2 2.977(4) . 4_666 no O1 O2 2.731(4) . 4_656 no O2 C1 3.367(5) . 5_564 no O2 N1 3.213(4) . 5_564 no O2 N2 3.065(4) . . no O3 N2 3.066(5) . 5_565 no O3 N1 3.041(4) . 1_545 no N1 N2 3.124(4) . 4_666 no N1 C2 2.453(5) . . no N1 N2 2.789(5) . . no N1 C3 3.418(5) . 1_565 no N2 C1 2.458(5) . . no N2 C3 3.386(5) . . no C1 C3 3.580(6) . 1_565 no C2 C3 3.542(5) . . no C2 C3 3.578(5) . 1_565 no C51 C51 3.418(18) . 6_655 no C62 C62 3.53(2) . 6_656 no _iucr_refine_instruction_details_constraints ; # # Punched on 21/05/15 at 10:49:12 # #LIST 12 BLOCK SCALE X'S, U'S CONT C(51,OCC) C(52,OCC) C(61,OCC) C(62,OCC) CONT H(11,X'S) UNTIL H(22) H(811,X'S) UNTIL H(912) SUMFIX ELEMENT SCALES EQUIV C(51,OCC) UNTIL C(62) WEIGHT -1 C(52,OCC) C(62,OCC) RIDE C ( 51,X'S) H ( 511,X'S) H ( 512,X'S) H ( 513,X'S) RIDE C ( 52,X'S) H ( 521,X'S) H ( 522,X'S) RIDE C ( 61,X'S) H ( 611,X'S) H ( 612,X'S) RIDE C ( 62,X'S) H ( 621,X'S) H ( 622,X'S) H ( 623,X'S) END ; _iucr_refine_instruction_details_restraints ; # # Punched on 21/05/15 at 10:49:12 # #LIST 16 DIST 1.33, .02 = C(4) TO C(52), C(4) TO C(61) DIST 1.50, .02 = C(4) TO C(51), C(4) TO C(62) U(IJ) 0.0, .001 = C(51) TO C(52) U(IJ) 0.0, .001 = C(61) TO C(62) U(IJ) 0.0, .01 = C(4) TO C(51) U(IJ) 0.0, .01 = C(4) TO C(52) U(IJ) 0.0, .01 = C(4) TO C(61) U(IJ) 0.0, .01 = C(4) TO C(62) ANGLE 0.0, 1 = MEAN C(3) TO C(4) TO C(51), C(3) TO C(4) TO C(62) ANGLE 0.0, 1 = MEAN C(3) TO C(4) TO C(52), C(3) TO C(4) TO C(61) ANGLE 0.0, 1 = MEAN C(51) TO C(4) TO C(61), C(52) TO C(4) TO C(62) REM HREST START (DO NOT REMOVE THIS LINE) REM HREST END (DO NOT REMOVE THIS LINE) END ; #===END