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#$Date: 2021-12-06 10:59:38 +0200 (Mon, 06 Dec 2021) $
#$Revision: 271126 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/55/1565551.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.
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data_1565551
loop_
_publ_author_name
'López Plá, Jessica M.'
'Boudalis, Athanassios K.'
'Telser, Joshua'
'Raptis, Raphael G.'
_publ_section_title
;
 Chromium(III)-pyrazole complexes. X-Ray crystal structures, 1H NMR
 investigation of ligand fluxional behavior and EPR studies
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119299
_journal_paper_doi               10.1016/j.ica.2019.119299
_journal_volume                  502
_journal_year                    2020
_chemical_formula_moiety         'C9 H9 Br3 Cl3 Cr N6'
_chemical_formula_sum            'C9 H9 Br3 Cl3 Cr N6'
_chemical_formula_weight         599.30
_chemical_name_systematic        mer-CrCl3(4-Br-pzH)3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 100.469(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.868(6)
_cell_length_b                   9.913(6)
_cell_length_c                   20.661(12)
_cell_measurement_reflns_used    7813
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      3.11
_cell_volume                     1786.0(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28963
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.476
_diffrn_reflns_theta_min         2.871
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.803
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4476
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1314 before and 0.0573 after correction. The Ratio of minimum to maximum transmission is 0.6005. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.239
_exptl_crystal_size_mid          0.172
_exptl_crystal_size_min          0.027
_refine_diff_density_max         0.791
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0373P)²+4.7086P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2962
_reflns_number_total             3678
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ICA-2020-502-119299.cif
_cod_data_source_block           jlp089_a
_cod_original_cell_volume        1785.9(18)
_cod_database_code               1565551
_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   0.817
_shelx_estimated_absorpt_t_min   0.257
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C1(H1), C3(H3), C4(H4A), C6(H6A), C7(H7), C9(H9)
;
_olex2_submission_original_sample_id JLP526
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Br1 Br 0.17462(7) 1.15253(5) 0.08790(3) 0.06353(18) Uani 1 1 d . . . . .
Br2 Br 0.18269(6) 0.99382(5) 0.47085(2) 0.05050(15) Uani 1 1 d . . . . .
Br3 Br 0.50994(7) 0.29826(6) 0.47805(3) 0.06822(19) Uani 1 1 d . . . . .
Cr1 Cr 0.25663(7) 0.63698(6) 0.24187(3) 0.02538(15) Uani 1 1 d . . . . .
Cl1 Cl 0.51477(11) 0.66067(10) 0.23962(5) 0.0361(2) Uani 1 1 d . . . . .
Cl2 Cl 0.22765(12) 0.47109(10) 0.16066(5) 0.0393(2) Uani 1 1 d . . . . .
Cl3 Cl -0.00222(11) 0.62330(11) 0.24653(6) 0.0401(3) Uani 1 1 d . . . . .
N1 N 0.2062(4) 0.7842(3) 0.17025(16) 0.0305(7) Uani 1 1 d . . . . .
N2 N 0.1426(6) 0.7543(4) 0.1083(2) 0.0608(13) Uani 1 1 d . . . . .
H2 H 0.118860 0.674103 0.094153 0.073 Uiso 1 1 calc R . . . .
N3 N 0.2832(4) 0.7834(3) 0.31595(16) 0.0292(7) Uani 1 1 d . . . . .
N4 N 0.4149(4) 0.8538(3) 0.33625(17) 0.0332(8) Uani 1 1 d . . . . .
H4 H 0.494715 0.848016 0.318177 0.040 Uiso 1 1 calc R . . . .
N5 N 0.3015(4) 0.4906(3) 0.31369(17) 0.0315(7) Uani 1 1 d . . . . .
N6 N 0.2160(4) 0.3790(3) 0.31306(19) 0.0390(9) Uani 1 1 d . . . . .
H6 H 0.138726 0.360209 0.282813 0.047 Uiso 1 1 calc R . . . .
C1 C 0.1205(8) 0.8661(6) 0.0712(3) 0.0730(19) Uani 1 1 d . . . . .
H1 H 0.078028 0.870452 0.026678 0.088 Uiso 1 1 calc R . . . .
C2 C 0.1714(5) 0.9703(4) 0.1105(2) 0.0415(10) Uani 1 1 d . . . . .
C3 C 0.2231(5) 0.9158(4) 0.1719(2) 0.0364(9) Uani 1 1 d . . . . .
H3 H 0.264188 0.965292 0.209180 0.044 Uiso 1 1 calc R . . . .
C4 C 0.4053(5) 0.9326(4) 0.3875(2) 0.0381(10) Uani 1 1 d . . . . .
H4A H 0.481191 0.989731 0.409200 0.046 Uiso 1 1 calc R . . . .
C5 C 0.2627(5) 0.9137(4) 0.4021(2) 0.0333(9) Uani 1 1 d . . . . .
C6 C 0.1898(5) 0.8212(4) 0.3570(2) 0.0342(9) Uani 1 1 d . . . . .
H6A H 0.090370 0.789763 0.355254 0.041 Uiso 1 1 calc R . . . .
C7 C 0.2654(5) 0.3005(5) 0.3650(2) 0.0444(11) Uani 1 1 d . . . . .
H7 H 0.223930 0.218323 0.374572 0.053 Uiso 1 1 calc R . . . .
C8 C 0.3889(5) 0.3646(4) 0.4015(2) 0.0389(10) Uani 1 1 d . . . . .
C9 C 0.4080(5) 0.4820(4) 0.3678(2) 0.0368(10) Uani 1 1 d . . . . .
H9 H 0.484244 0.545746 0.381108 0.044 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'
Br Br -0.2901 2.4595 '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'
Cr Cr 0.3209 0.6236 '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'
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
Cl1 Cr1 Cl2 92.14(5) . .
Cl1 Cr1 Cl3 177.24(5) . .
Cl3 Cr1 Cl2 90.47(5) . .
N1 Cr1 Cl1 90.01(10) . .
N1 Cr1 Cl2 90.10(11) . .
N1 Cr1 Cl3 89.08(10) . .
N1 Cr1 N3 90.85(14) . .
N3 Cr1 Cl1 87.94(9) . .
N3 Cr1 Cl2 179.05(10) . .
N3 Cr1 Cl3 89.47(9) . .
N5 Cr1 Cl1 91.35(10) . .
N5 Cr1 Cl2 90.19(11) . .
N5 Cr1 Cl3 89.55(10) . .
N5 Cr1 N1 178.60(13) . .
N5 Cr1 N3 88.87(14) . .
N2 N1 Cr1 121.8(3) . .
C3 N1 Cr1 132.4(3) . .
C3 N1 N2 105.8(3) . .
N1 N2 H2 124.6 . .
N1 N2 C1 110.9(4) . .
C1 N2 H2 124.6 . .
N4 N3 Cr1 123.9(2) . .
C6 N3 Cr1 131.0(3) . .
C6 N3 N4 104.8(3) . .
N3 N4 H4 124.1 . .
C4 N4 N3 111.8(3) . .
C4 N4 H4 124.1 . .
N6 N5 Cr1 122.6(3) . .
C9 N5 Cr1 131.7(3) . .
C9 N5 N6 105.6(3) . .
N5 N6 H6 124.1 . .
C7 N6 N5 111.8(4) . .
C7 N6 H6 124.1 . .
N2 C1 H1 126.5 . .
C2 C1 N2 107.0(5) . .
C2 C1 H1 126.5 . .
C1 C2 Br1 127.8(4) . .
C1 C2 C3 105.9(4) . .
C3 C2 Br1 126.3(4) . .
N1 C3 C2 110.4(4) . .
N1 C3 H3 124.8 . .
C2 C3 H3 124.8 . .
N4 C4 H4A 126.5 . .
N4 C4 C5 106.9(4) . .
C5 C4 H4A 126.5 . .
C4 C5 Br2 127.1(3) . .
C4 C5 C6 106.3(4) . .
C6 C5 Br2 126.7(3) . .
N3 C6 C5 110.2(4) . .
N3 C6 H6A 124.9 . .
C5 C6 H6A 124.9 . .
N6 C7 H7 126.7 . .
N6 C7 C8 106.6(4) . .
C8 C7 H7 126.7 . .
C7 C8 Br3 125.7(3) . .
C7 C8 C9 105.8(4) . .
C9 C8 Br3 128.4(4) . .
N5 C9 C8 110.2(4) . .
N5 C9 H9 124.9 . .
C8 C9 H9 124.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 C2 1.868(4) .
Br2 C5 1.875(4) .
Br3 C8 1.863(4) .
Cr1 Cl1 2.3100(18) .
Cr1 Cl2 2.3300(15) .
Cr1 Cl3 2.3188(18) .
Cr1 N1 2.069(3) .
Cr1 N3 2.091(3) .
Cr1 N5 2.062(3) .
N1 N2 1.334(5) .
N1 C3 1.313(5) .
N2 H2 0.8600 .
N2 C1 1.342(7) .
N3 N4 1.360(4) .
N3 C6 1.341(5) .
N4 H4 0.8600 .
N4 C4 1.332(5) .
N5 N6 1.340(5) .
N5 C9 1.328(5) .
N6 H6 0.8600 .
N6 C7 1.333(6) .
C1 H1 0.9300 .
C1 C2 1.341(7) .
C2 C3 1.377(6) .
C3 H3 0.9300 .
C4 H4A 0.9300 .
C4 C5 1.365(6) .
C5 C6 1.382(6) .
C6 H6A 0.9300 .
C7 H7 0.9300 .
C7 C8 1.368(6) .
C8 C9 1.382(6) .
C9 H9 0.9300 .
