#------------------------------------------------------------------------------
#$Date: 2024-12-05 22:09:13 +0200 (Thu, 05 Dec 2024) $
#$Revision: 296231 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/16/02/7160280.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7160280
loop_
_publ_author_name
'Kukreti, Prashant'
'Chauhan, Rahul'
'Panwar, Abhishek'
'Ghosh, Kaushik'
_publ_section_title
;
 A multi-component synthetic route for 2-pyrazolines via
 acceptorless dehydrogenation of alcohols using homogeneous Ni(II)
 catalysts.
;
_journal_issue                   41
_journal_name_full               'Organic & biomolecular chemistry'
_journal_page_first              8273
_journal_page_last               8278
_journal_paper_doi               10.1039/d4ob01352b
_journal_volume                  22
_journal_year                    2024
_chemical_formula_moiety         'C35 H27 Cl2 N7 Ni'
_chemical_formula_sum            'C35 H27 Cl2 N7 Ni'
_chemical_formula_weight         675.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-16
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-09-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.322(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7783(11)
_cell_length_b                   12.1608(6)
_cell_length_c                   26.3729(12)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      24.845
_cell_measurement_theta_min      2.317
_cell_volume                     6657.0(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker Instrument Service vV6.2.16'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      115.0
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0885
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            244773
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.358
_diffrn_reflns_theta_min         2.296
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1347 before and 0.0734 after correction. The Ratio of minimum to maximum transmission is 0.9021. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'metallic yellowish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             2784
_exptl_crystal_size_max          0.105
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.026
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     823
_refine_ls_number_reflns         16576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0515
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0536P)²+10.6823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12775
_reflns_number_total             16576
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ob01352b2.cif
_cod_data_source_block           testrun_71_0m_a
_cod_database_code               7160280
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
  C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23),
 C24(H24), C25(H25), C26(H26), C27(H27), C31(H31), C32(H32), C33(H33), C34(H34),
  C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
 C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55),
  C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C66(H66),
 C67(H67), C68(H68), C69(H69), C70(H70)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.65007(2) 0.72601(3) 0.20343(2) 0.01573(8) Uani 1 1 d . . . . .
Ni2 Ni 0.34899(2) 0.53759(3) 0.29902(2) 0.01949(8) Uani 1 1 d . . . . .
Cl1 Cl 0.56891(3) 0.61138(6) 0.15453(3) 0.02480(14) Uani 1 1 d . . . . .
Cl2 Cl 0.75846(3) 0.73650(5) 0.26379(3) 0.01947(13) Uani 1 1 d . . . . .
Cl3 Cl 0.43087(3) 0.65431(6) 0.34265(3) 0.02909(16) Uani 1 1 d . . . . .
Cl4 Cl 0.23910(3) 0.52513(5) 0.24325(3) 0.02110(13) Uani 1 1 d . . . . .
N1 N 0.67258(12) 0.39853(19) 0.29226(10) 0.0230(5) Uani 1 1 d . . . . .
H1 H 0.6924(16) 0.351(3) 0.2811(14) 0.034 Uiso 1 1 d R . . . .
N2 N 0.37460(11) 0.50443(18) 0.23227(10) 0.0218(5) Uani 1 1 d . . . . .
N3 N 0.71908(12) 0.4282(2) 0.14302(10) 0.0245(5) Uani 1 1 d . . . . .
H3 H 0.7335(17) 0.374(3) 0.1643(15) 0.037 Uiso 1 1 d R . . . .
N4 N 0.62303(11) 0.74520(17) 0.27018(9) 0.0181(4) Uani 1 1 d . . . . .
N5 N 0.63030(11) 0.88181(17) 0.19838(9) 0.0174(4) Uani 1 1 d . . . . .
N6 N 0.60904(11) 0.85576(17) 0.27502(9) 0.0199(5) Uani 1 1 d . . . . .
N7 N 0.66647(11) 0.77106(17) 0.13313(9) 0.0186(4) Uani 1 1 d . . . . .
N8 N 0.65630(12) 0.88417(18) 0.12321(9) 0.0211(5) Uani 1 1 d . . . . .
N9 N 0.27389(12) 0.8518(2) 0.35381(10) 0.0264(5) Uani 1 1 d . . . . .
H9A H 0.2696(17) 0.906(3) 0.3301(15) 0.040 Uiso 1 1 d R . . . .
N10 N 0.33155(11) 0.50681(18) 0.37088(9) 0.0217(5) Uani 1 1 d . . . . .
N11 N 0.37151(11) 0.38368(18) 0.31089(10) 0.0219(5) Uani 1 1 d . . . . .
N12 N 0.34523(12) 0.39563(19) 0.38609(10) 0.0266(5) Uani 1 1 d . . . . .
N13 N 0.39491(12) 0.39541(18) 0.23431(10) 0.0252(5) Uani 1 1 d . . . . .
N14 N 0.31591(12) 0.84308(19) 0.20213(10) 0.0213(5) Uani 1 1 d . . . . .
H14 H 0.2932(16) 0.888(3) 0.2098(14) 0.032 Uiso 1 1 d R . . . .
C1 C 0.60738(12) 0.4738(2) 0.32754(11) 0.0190(5) Uani 1 1 d . . . . .
C2 C 0.63392(13) 0.3743(2) 0.31950(11) 0.0203(5) Uani 1 1 d . . . . .
C3 C 0.62057(14) 0.2734(2) 0.33785(12) 0.0255(6) Uani 1 1 d . . . . .
H3A H 0.639715 0.207015 0.333078 0.031 Uiso 1 1 calc R . . . .
C4 C 0.57863(15) 0.2745(2) 0.36303(14) 0.0314(7) Uani 1 1 d . . . . .
H4 H 0.568652 0.207335 0.376117 0.038 Uiso 1 1 calc R . . . .
C5 C 0.54998(15) 0.3723(3) 0.37004(13) 0.0305(7) Uani 1 1 d . . . . .
H5 H 0.520441 0.369608 0.387016 0.037 Uiso 1 1 calc R . . . .
C6 C 0.56392(13) 0.4720(2) 0.35274(12) 0.0234(6) Uani 1 1 d . . . . .
H6 H 0.544542 0.537863 0.357779 0.028 Uiso 1 1 calc R . . . .
C7 C 0.63173(13) 0.5596(2) 0.30373(11) 0.0208(5) Uani 1 1 d . . . . .
C8 C 0.67143(14) 0.5084(2) 0.28314(12) 0.0246(6) Uani 1 1 d . . . . .
H8 H 0.694554 0.544754 0.265202 0.030 Uiso 1 1 calc R . . . .
C9 C 0.61540(13) 0.6742(2) 0.30316(11) 0.0213(5) Uani 1 1 d . . . . .
H9 H 0.598108 0.698589 0.328407 0.026 Uiso 1 1 calc R . . . .
C10 C 0.61184(12) 0.9271(2) 0.23553(10) 0.0174(5) Uani 1 1 d . . . . .
C11 C 0.59630(13) 1.0385(2) 0.23311(11) 0.0192(5) Uani 1 1 d . . . . .
H11 H 0.582942 1.071150 0.259354 0.023 Uiso 1 1 calc R . . . .
C12 C 0.60126(13) 1.0992(2) 0.19080(11) 0.0214(5) Uani 1 1 d . . . . .
H12 H 0.591254 1.175384 0.188236 0.026 Uiso 1 1 calc R . . . .
C13 C 0.62034(13) 1.0529(2) 0.15182(11) 0.0212(5) Uani 1 1 d . . . . .
H13 H 0.623209 1.095410 0.122699 0.025 Uiso 1 1 calc R . . . .
C14 C 0.63502(12) 0.9415(2) 0.15747(11) 0.0185(5) Uani 1 1 d . . . . .
C15 C 0.58488(13) 0.8921(2) 0.31496(11) 0.0187(5) Uani 1 1 d . . . . .
C16 C 0.62598(14) 0.9490(2) 0.36214(11) 0.0229(6) Uani 1 1 d . . . . .
H16 H 0.669723 0.961318 0.368785 0.027 Uiso 1 1 calc R . . . .
C17 C 0.60158(14) 0.9872(2) 0.39922(12) 0.0262(6) Uani 1 1 d . . . . .
H17 H 0.628713 1.026528 0.431496 0.031 Uiso 1 1 calc R . . . .
C18 C 0.53816(15) 0.9682(2) 0.38934(12) 0.0254(6) Uani 1 1 d . . . . .
H18 H 0.521777 0.995147 0.414764 0.031 Uiso 1 1 calc R . . . .
C19 C 0.49806(14) 0.9101(2) 0.34277(12) 0.0239(6) Uani 1 1 d . . . . .
H19 H 0.454608 0.896328 0.336666 0.029 Uiso 1 1 calc R . . . .
C20 C 0.52145(13) 0.8722(2) 0.30501(11) 0.0205(5) Uani 1 1 d . . . . .
H20 H 0.494132 0.833067 0.272720 0.025 Uiso 1 1 calc R . . . .
C21 C 0.65699(14) 0.9336(2) 0.07398(11) 0.0213(5) Uani 1 1 d . . . . .
C22 C 0.60004(15) 0.9449(3) 0.02715(12) 0.0286(6) Uani 1 1 d . . . . .
H22 H 0.560491 0.919959 0.027103 0.034 Uiso 1 1 calc R . . . .
C23 C 0.60179(17) 0.9936(3) -0.02005(12) 0.0352(7) Uani 1 1 d . . . . .
H23 H 0.562965 1.002342 -0.052509 0.042 Uiso 1 1 calc R . . . .
C24 C 0.65901(16) 1.0293(2) -0.02021(12) 0.0300(7) Uani 1 1 d . . . . .
H24 H 0.659539 1.062811 -0.052557 0.036 Uiso 1 1 calc R . . . .
C25 C 0.71547(16) 1.0163(2) 0.02652(13) 0.0298(7) Uani 1 1 d . . . . .
H25 H 0.755110 1.039840 0.026244 0.036 Uiso 1 1 calc R . . . .
C26 C 0.71461(15) 0.9689(2) 0.07410(12) 0.0251(6) Uani 1 1 d . . . . .
H26 H 0.753489 0.960714 0.106555 0.030 Uiso 1 1 calc R . . . .
C27 C 0.67390(13) 0.7105(2) 0.09619(11) 0.0216(5) Uani 1 1 d . . . . .
H27 H 0.670757 0.743219 0.062459 0.026 Uiso 1 1 calc R . . . .
C28 C 0.68687(14) 0.5940(2) 0.10460(11) 0.0210(5) Uani 1 1 d . . . . .
C29 C 0.66206(14) 0.5123(2) 0.06129(12) 0.0248(6) Uani 1 1 d . . . . .
C30 C 0.68308(14) 0.4097(2) 0.08700(12) 0.0253(6) Uani 1 1 d . . . . .
C31 C 0.72099(13) 0.5384(2) 0.15370(11) 0.0215(5) Uani 1 1 d . . . . .
H31 H 0.742386 0.571583 0.189245 0.026 Uiso 1 1 calc R . . . .
C32 C 0.62215(16) 0.5169(3) 0.00436(12) 0.0320(7) Uani 1 1 d . . . . .
H32 H 0.605982 0.585214 -0.013353 0.038 Uiso 1 1 calc R . . . .
C33 C 0.60683(18) 0.4199(3) -0.02546(14) 0.0415(8) Uani 1 1 d . . . . .
H33 H 0.580235 0.421735 -0.064222 0.050 Uiso 1 1 calc R . . . .
C34 C 0.62998(19) 0.3184(3) 0.00065(16) 0.0457(9) Uani 1 1 d . . . . .
H34 H 0.619060 0.253063 -0.021014 0.055 Uiso 1 1 calc R . . . .
C35 C 0.66793(17) 0.3113(3) 0.05661(15) 0.0370(8) Uani 1 1 d . . . . .
H35 H 0.683315 0.242430 0.074069 0.044 Uiso 1 1 calc R . . . .
C36 C 0.28458(13) 0.7542(2) 0.42982(11) 0.0233(6) Uani 1 1 d . . . . .
C37 C 0.27107(14) 0.8591(2) 0.40500(12) 0.0246(6) Uani 1 1 d . . . . .
C38 C 0.25663(15) 0.9501(2) 0.43023(12) 0.0287(6) Uani 1 1 d . . . . .
H38 H 0.247870 1.020121 0.412755 0.034 Uiso 1 1 calc R . . . .
C39 C 0.25566(15) 0.9336(3) 0.48149(13) 0.0319(7) Uani 1 1 d . . . . .
H39 H 0.245650 0.993173 0.499832 0.038 Uiso 1 1 calc R . . . .
C40 C 0.26933(15) 0.8294(3) 0.50713(13) 0.0317(7) Uani 1 1 d . . . . .
H40 H 0.268397 0.820298 0.542563 0.038 Uiso 1 1 calc R . . . .
C41 C 0.28394(14) 0.7409(3) 0.48226(12) 0.0274(6) Uani 1 1 d . . . . .
H41 H 0.293491 0.671454 0.500389 0.033 Uiso 1 1 calc R . . . .
C42 C 0.29613(14) 0.6829(2) 0.39116(11) 0.0239(6) Uani 1 1 d . . . . .
C43 C 0.28872(14) 0.7470(2) 0.34568(12) 0.0263(6) Uani 1 1 d . . . . .
H43 H 0.293320 0.721448 0.313462 0.032 Uiso 1 1 calc R . . . .
C44 C 0.31343(14) 0.5679(2) 0.40198(11) 0.0245(6) Uani 1 1 d . . . . .
H44 H 0.311322 0.535242 0.433923 0.029 Uiso 1 1 calc R . . . .
C45 C 0.36716(13) 0.3316(2) 0.35417(11) 0.0225(6) Uani 1 1 d . . . . .
C46 C 0.38291(14) 0.2213(2) 0.36458(12) 0.0263(6) Uani 1 1 d . . . . .
H46 H 0.379317 0.183878 0.394800 0.032 Uiso 1 1 calc R . . . .
C47 C 0.40413(14) 0.1683(2) 0.32877(12) 0.0266(6) Uani 1 1 d . . . . .
H47 H 0.415050 0.092523 0.334728 0.032 Uiso 1 1 calc R . . . .
C48 C 0.41006(14) 0.2211(2) 0.28469(12) 0.0246(6) Uani 1 1 d . . . . .
H48 H 0.425473 0.183790 0.260936 0.030 Uiso 1 1 calc R . . . .
C49 C 0.39241(13) 0.3314(2) 0.27672(11) 0.0219(6) Uani 1 1 d . . . . .
C50 C 0.34521(15) 0.3529(2) 0.43697(11) 0.0269(6) Uani 1 1 d . . . . .
C51 C 0.29112(17) 0.3039(3) 0.43703(13) 0.0327(7) Uani 1 1 d . . . . .
H51 H 0.253023 0.299951 0.403592 0.039 Uiso 1 1 calc R . . . .
C52 C 0.2919(2) 0.2600(3) 0.48597(16) 0.0492(10) Uani 1 1 d . . . . .
H52 H 0.254679 0.224662 0.485994 0.059 Uiso 1 1 calc R . . . .
C53 C 0.3465(3) 0.2681(3) 0.53395(16) 0.0569(12) Uani 1 1 d . . . . .
H53 H 0.346571 0.239257 0.567474 0.068 Uiso 1 1 calc R . . . .
C54 C 0.4011(2) 0.3167(4) 0.53487(14) 0.0572(12) Uani 1 1 d . . . . .
H54 H 0.438991 0.320037 0.568477 0.069 Uiso 1 1 calc R . . . .
C55 C 0.40050(18) 0.3617(3) 0.48551(14) 0.0409(8) Uani 1 1 d . . . . .
H55 H 0.437549 0.397709 0.485573 0.049 Uiso 1 1 calc R . . . .
C56 C 0.41803(14) 0.3538(2) 0.19461(12) 0.0230(6) Uani 1 1 d . . . . .
C57 C 0.47693(14) 0.3874(2) 0.19688(13) 0.0277(6) Uani 1 1 d . . . . .
H57 H 0.504047 0.433734 0.226155 0.033 Uiso 1 1 calc R . . . .
C58 C 0.49605(15) 0.3527(2) 0.15601(14) 0.0313(7) Uani 1 1 d . . . . .
H58 H 0.535976 0.376904 0.156604 0.038 Uiso 1 1 calc R . . . .
C59 C 0.45710(17) 0.2828(2) 0.11425(13) 0.0323(7) Uani 1 1 d . . . . .
H59 H 0.470495 0.258775 0.086388 0.039 Uiso 1 1 calc R . . . .
C60 C 0.39909(15) 0.2480(2) 0.11303(12) 0.0298(7) Uani 1 1 d . . . . .
H60 H 0.372697 0.199462 0.084529 0.036 Uiso 1 1 calc R . . . .
C61 C 0.37900(14) 0.2835(2) 0.15319(13) 0.0258(6) Uani 1 1 d . . . . .
H61 H 0.338860 0.259792 0.152337 0.031 Uiso 1 1 calc R . . . .
C62 C 0.37692(14) 0.5688(2) 0.19428(12) 0.0228(6) Uani 1 1 d . . . . .
H62 H 0.391523 0.540566 0.167914 0.027 Uiso 1 1 calc R . . . .
C63 C 0.35787(13) 0.6827(2) 0.19083(11) 0.0210(5) Uani 1 1 d . . . . .
C64 C 0.39009(13) 0.7716(2) 0.17585(10) 0.0191(5) Uani 1 1 d . . . . .
C65 C 0.36317(13) 0.8697(2) 0.18465(11) 0.0199(5) Uani 1 1 d . . . . .
C66 C 0.31299(14) 0.7317(2) 0.20638(12) 0.0230(6) Uani 1 1 d . . . . .
H66 H 0.284456 0.693551 0.218217 0.028 Uiso 1 1 calc R . . . .
C67 C 0.44032(13) 0.7753(2) 0.15885(11) 0.0215(5) Uani 1 1 d . . . . .
H67 H 0.458847 0.709660 0.152460 0.026 Uiso 1 1 calc R . . . .
C68 C 0.46252(13) 0.8774(2) 0.15151(11) 0.0243(6) Uani 1 1 d . . . . .
H68 H 0.496549 0.881667 0.139614 0.029 Uiso 1 1 calc R . . . .
C69 C 0.43569(14) 0.9747(2) 0.16131(12) 0.0269(6) Uani 1 1 d . . . . .
H69 H 0.452563 1.043453 0.156565 0.032 Uiso 1 1 calc R . . . .
C70 C 0.38577(14) 0.9730(2) 0.17756(11) 0.0220(6) Uani 1 1 d . . . . .
H70 H 0.367352 1.038940 0.183728 0.026 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Ni1 Cl2 144.74(3) . . ?
N4 Ni1 Cl1 95.38(6) . . ?
N4 Ni1 Cl2 90.88(6) . . ?
N4 Ni1 N7 157.78(8) . . ?
N5 Ni1 Cl1 116.96(7) . . ?
N5 Ni1 Cl2 98.30(7) . . ?
N5 Ni1 N4 79.01(9) . . ?
N5 Ni1 N7 78.81(9) . . ?
N7 Ni1 Cl1 93.34(6) . . ?
N7 Ni1 Cl2 93.72(6) . . ?
Cl3 Ni2 Cl4 144.52(3) . . ?
N2 Ni2 Cl3 95.26(7) . . ?
N2 Ni2 Cl4 93.17(7) . . ?
N2 Ni2 N10 158.27(9) . . ?
N10 Ni2 Cl3 94.31(7) . . ?
N10 Ni2 Cl4 90.27(7) . . ?
N11 Ni2 Cl3 114.84(7) . . ?
N11 Ni2 Cl4 100.60(7) . . ?
N11 Ni2 N2 78.68(9) . . ?
N11 Ni2 N10 79.60(9) . . ?
C8 N1 C2 109.5(2) . . ?
N13 N2 Ni2 110.49(17) . . ?
C62 N2 Ni2 130.26(19) . . ?
C62 N2 N13 119.1(2) . . ?
C31 N3 C30 109.5(2) . . ?
N6 N4 Ni1 109.82(15) . . ?
C9 N4 Ni1 131.19(18) . . ?
C9 N4 N6 118.9(2) . . ?
C10 N5 Ni1 119.18(17) . . ?
C10 N5 C14 121.4(2) . . ?
C14 N5 Ni1 119.39(17) . . ?
N4 N6 C15 122.0(2) . . ?
C10 N6 N4 117.0(2) . . ?
C10 N6 C15 120.6(2) . . ?
N8 N7 Ni1 110.10(15) . . ?
C27 N7 Ni1 130.01(18) . . ?
C27 N7 N8 118.9(2) . . ?
N7 N8 C21 121.1(2) . . ?
C14 N8 N7 116.7(2) . . ?
C14 N8 C21 121.3(2) . . ?
C43 N9 C37 109.2(2) . . ?
N12 N10 Ni2 108.81(16) . . ?
C44 N10 Ni2 133.67(19) . . ?
C44 N10 N12 117.5(2) . . ?
C45 N11 Ni2 119.11(19) . . ?
C49 N11 Ni2 119.63(18) . . ?
C49 N11 C45 121.2(2) . . ?
N10 N12 C50 121.8(2) . . ?
C45 N12 N10 117.4(2) . . ?
C45 N12 C50 120.2(2) . . ?
N2 N13 C56 121.2(2) . . ?
C49 N13 N2 116.2(2) . . ?
C49 N13 C56 122.6(2) . . ?
C66 N14 C65 109.5(2) . . ?
C2 C1 C7 106.9(2) . . ?
C6 C1 C2 119.3(2) . . ?
C6 C1 C7 133.8(2) . . ?
N1 C2 C1 107.5(2) . . ?
N1 C2 C3 130.2(3) . . ?
C3 C2 C1 122.3(3) . . ?
C4 C3 C2 117.0(3) . . ?
C3 C4 C5 121.8(3) . . ?
C6 C5 C4 121.2(3) . . ?
C5 C6 C1 118.4(3) . . ?
C8 C7 C1 106.1(2) . . ?
C8 C7 C9 129.9(2) . . ?
C9 C7 C1 124.1(2) . . ?
N1 C8 C7 110.1(2) . . ?
N4 C9 C7 123.3(2) . . ?
N5 C10 N6 115.0(2) . . ?
N5 C10 C11 121.2(2) . . ?
N6 C10 C11 123.8(2) . . ?
C12 C11 C10 116.9(2) . . ?
C11 C12 C13 122.4(2) . . ?
C14 C13 C12 116.8(2) . . ?
N5 C14 N8 114.9(2) . . ?
N5 C14 C13 121.3(2) . . ?
N8 C14 C13 123.9(2) . . ?
C16 C15 N6 119.0(2) . . ?
C20 C15 N6 119.5(2) . . ?
C20 C15 C16 121.5(2) . . ?
C17 C16 C15 118.6(3) . . ?
C18 C17 C16 120.2(3) . . ?
C17 C18 C19 120.7(3) . . ?
C18 C19 C20 119.9(3) . . ?
C15 C20 C19 119.1(2) . . ?
C22 C21 N8 119.6(3) . . ?
C26 C21 N8 119.5(2) . . ?
C26 C21 C22 120.9(2) . . ?
C21 C22 C23 118.6(3) . . ?
C24 C23 C22 120.8(3) . . ?
C23 C24 C25 119.9(3) . . ?
C24 C25 C26 120.1(3) . . ?
C21 C26 C25 119.7(3) . . ?
N7 C27 C28 121.8(2) . . ?
C29 C28 C27 124.4(2) . . ?
C31 C28 C27 128.6(3) . . ?
C31 C28 C29 106.9(2) . . ?
C30 C29 C28 106.6(2) . . ?
C32 C29 C28 133.7(3) . . ?
C32 C29 C30 119.6(3) . . ?
N3 C30 C29 107.8(2) . . ?
N3 C30 C35 130.4(3) . . ?
C35 C30 C29 121.8(3) . . ?
N3 C31 C28 109.2(2) . . ?
C33 C32 C29 118.5(3) . . ?
C32 C33 C34 121.0(3) . . ?
C35 C34 C33 121.7(3) . . ?
C34 C35 C30 117.3(3) . . ?
C37 C36 C42 106.5(2) . . ?
C41 C36 C37 118.4(3) . . ?
C41 C36 C42 135.1(3) . . ?
N9 C37 C36 107.9(2) . . ?
N9 C37 C38 129.1(3) . . ?
C38 C37 C36 123.0(3) . . ?
C39 C38 C37 117.0(3) . . ?
C38 C39 C40 120.9(3) . . ?
C41 C40 C39 121.7(3) . . ?
C40 C41 C36 119.0(3) . . ?
C36 C42 C44 123.7(3) . . ?
C43 C42 C36 106.4(2) . . ?
C43 C42 C44 129.9(3) . . ?
N9 C43 C42 110.0(3) . . ?
N10 C44 C42 124.1(3) . . ?
N11 C45 N12 115.1(2) . . ?
N11 C45 C46 121.3(3) . . ?
N12 C45 C46 123.6(3) . . ?
C47 C46 C45 116.7(3) . . ?
C48 C47 C46 122.7(3) . . ?
C47 C48 C49 116.9(3) . . ?
N11 C49 N13 114.9(2) . . ?
N11 C49 C48 121.1(3) . . ?
N13 C49 C48 124.0(3) . . ?
C51 C50 N12 120.3(3) . . ?
C51 C50 C55 120.7(3) . . ?
C55 C50 N12 119.0(3) . . ?
C50 C51 C52 120.1(3) . . ?
C53 C52 C51 119.4(4) . . ?
C52 C53 C54 121.5(3) . . ?
C53 C54 C55 119.3(4) . . ?
C50 C55 C54 119.0(4) . . ?
C57 C56 N13 120.2(3) . . ?
C57 C56 C61 120.9(3) . . ?
C61 C56 N13 118.8(3) . . ?
C56 C57 C58 119.2(3) . . ?
C57 C58 C59 120.2(3) . . ?
C60 C59 C58 120.1(3) . . ?
C59 C60 C61 120.2(3) . . ?
C56 C61 C60 119.3(3) . . ?
N2 C62 C63 121.6(2) . . ?
C62 C63 C64 124.0(2) . . ?
C66 C63 C62 129.4(2) . . ?
C66 C63 C64 106.2(2) . . ?
C65 C64 C63 106.5(2) . . ?
C67 C64 C63 133.5(2) . . ?
C67 C64 C65 119.9(2) . . ?
N14 C65 C64 108.1(2) . . ?
N14 C65 C70 129.8(2) . . ?
C70 C65 C64 122.1(2) . . ?
N14 C66 C63 109.7(2) . . ?
C68 C67 C64 118.1(3) . . ?
C67 C68 C69 121.2(3) . . ?
C70 C69 C68 121.7(3) . . ?
C69 C70 C65 117.0(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Cl1 2.2495(7) . ?
Ni1 Cl2 2.3256(7) . ?
Ni1 N4 2.104(2) . ?
Ni1 N5 1.939(2) . ?
Ni1 N7 2.109(2) . ?
Ni2 Cl3 2.2470(8) . ?
Ni2 Cl4 2.3280(7) . ?
Ni2 N2 2.109(2) . ?
Ni2 N10 2.124(2) . ?
Ni2 N11 1.932(2) . ?
N1 C2 1.378(4) . ?
N1 C8 1.355(4) . ?
N2 N13 1.398(3) . ?
N2 C62 1.290(4) . ?
N3 C30 1.381(4) . ?
N3 C31 1.367(4) . ?
N4 N6 1.400(3) . ?
N4 C9 1.287(3) . ?
N5 C10 1.334(3) . ?
N5 C14 1.341(3) . ?
N6 C10 1.377(3) . ?
N6 C15 1.444(3) . ?
N7 N8 1.401(3) . ?
N7 C27 1.287(3) . ?
N8 C14 1.378(3) . ?
N8 C21 1.436(3) . ?
N9 C37 1.381(4) . ?
N9 C43 1.359(4) . ?
N10 N12 1.408(3) . ?
N10 C44 1.293(4) . ?
N11 C45 1.344(3) . ?
N11 C49 1.340(4) . ?
N12 C45 1.382(4) . ?
N12 C50 1.439(4) . ?
N13 C49 1.383(4) . ?
N13 C56 1.444(4) . ?
N14 C65 1.373(3) . ?
N14 C66 1.363(3) . ?
C1 C2 1.407(4) . ?
C1 C6 1.402(4) . ?
C1 C7 1.441(4) . ?
C2 C3 1.398(4) . ?
C3 C4 1.370(4) . ?
C4 C5 1.405(4) . ?
C5 C6 1.378(4) . ?
C7 C8 1.380(4) . ?
C7 C9 1.441(4) . ?
C10 C11 1.395(4) . ?
C11 C12 1.380(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.389(4) . ?
C15 C16 1.394(4) . ?
C15 C20 1.379(4) . ?
C16 C17 1.389(4) . ?
C17 C18 1.378(4) . ?
C18 C19 1.385(4) . ?
C19 C20 1.388(4) . ?
C21 C22 1.381(4) . ?
C21 C26 1.380(4) . ?
C22 C23 1.394(4) . ?
C23 C24 1.375(5) . ?
C24 C25 1.376(4) . ?
C25 C26 1.389(4) . ?
C27 C28 1.445(4) . ?
C28 C29 1.443(4) . ?
C28 C31 1.382(4) . ?
C29 C30 1.407(4) . ?
C29 C32 1.400(4) . ?
C30 C35 1.402(4) . ?
C32 C33 1.381(4) . ?
C33 C34 1.406(5) . ?
C34 C35 1.372(5) . ?
C36 C37 1.409(4) . ?
C36 C41 1.398(4) . ?
C36 C42 1.442(4) . ?
C37 C38 1.398(4) . ?
C38 C39 1.376(4) . ?
C39 C40 1.409(5) . ?
C40 C41 1.371(4) . ?
C42 C43 1.381(4) . ?
C42 C44 1.450(4) . ?
C45 C46 1.387(4) . ?
C46 C47 1.384(4) . ?
C47 C48 1.383(4) . ?
C48 C49 1.392(4) . ?
C50 C51 1.369(5) . ?
C50 C55 1.381(4) . ?
C51 C52 1.390(4) . ?
C52 C53 1.364(6) . ?
C53 C54 1.369(7) . ?
C54 C55 1.407(6) . ?
C56 C57 1.380(4) . ?
C56 C61 1.384(4) . ?
C57 C58 1.384(4) . ?
C58 C59 1.385(5) . ?
C59 C60 1.375(5) . ?
C60 C61 1.384(4) . ?
C62 C63 1.443(4) . ?
C63 C64 1.449(4) . ?
C63 C66 1.384(4) . ?
C64 C65 1.404(4) . ?
C64 C67 1.391(4) . ?
C65 C70 1.398(4) . ?
C67 C68 1.384(4) . ?
C68 C69 1.404(4) . ?
C69 C70 1.371(4) . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.984 0.000 234.5 66.4 ?
2 0.000 0.000 0.500 118.4 17.0 ?
3 0.500 -0.672 0.500 234.5 66.4 ?
4 0.500 0.500 1.000 118.4 17.0 ?
