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#$Date: 2022-09-08 02:04:43 +0300 (Thu, 08 Sep 2022) $
#$Revision: 277723 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/11/7711196.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_7711196
loop_
_publ_author_name
'Herrera, Susana'
'Rivero, Kennett I.'
'Guzmán, Alexis'
'Cedeño, Jonathan'
'Miksovska, Jaroslava'
'Raptis, Raphael G.'
_publ_section_title
;
 Mononuclear, hexanuclear and polymeric indium(iii) pyrazolido complexes;
 structural characterization, dynamic solution studies and luminescent
 properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01901A
_journal_year                    2022
_chemical_formula_moiety         'C9 H9 Cl6 In N6'
_chemical_formula_sum            'C9 H9 Cl6 In N6'
_chemical_formula_weight         528.74
_chemical_name_common            mer-[InCl3(4-Cl-pzH)3]
_chemical_name_systematic        InCl3(N2C3ClH3)3
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-11-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                78.541(5)
_cell_angle_beta                 89.430(5)
_cell_angle_gamma                87.010(5)
_cell_formula_units_Z            2
_cell_length_a                   6.8851(11)
_cell_length_b                   10.5525(18)
_cell_length_c                   12.437(2)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    296
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.83
_cell_volume                     884.4(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296
_diffrn_detector_type            'Photon 100 Detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12966
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.099
_diffrn_reflns_theta_min         2.827
_exptl_absorpt_coefficient_mu    2.244
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6611
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0660 before and 0.0412 after correction.
The Ratio of minimum to maximum transmission is 0.8865.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.986
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.236
_exptl_crystal_size_min          0.233
_refine_diff_density_max         0.749
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0294(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0238
_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)+(0.0191P)²+0.9542P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0540
_refine_ls_wR_factor_ref         0.0554
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3643
_reflns_number_total             3883
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01901a2.cif
_cod_data_source_block           sh030_0m_a
_cod_database_code               7711196
_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   0.623
_shelx_estimated_absorpt_t_min   0.511
_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:
 N4(H4), N6(H6), C4(H4A), C6(H6A), C3(H3), C1(H1), C7(H7), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_original_sample_id SH203
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
In1 In 0.16948(2) 0.32089(2) 0.79814(2) 0.03029(7) Uani 1 1 d . . . . .
Cl6 Cl 0.42910(9) 0.18503(7) 0.90188(5) 0.04287(15) Uani 1 1 d . . . . .
Cl5 Cl -0.03780(10) 0.33630(7) 0.95723(6) 0.04576(16) Uani 1 1 d . . . . .
Cl4 Cl -0.05797(10) 0.46153(7) 0.66805(6) 0.04645(16) Uani 1 1 d . . . . .
Cl2 Cl 0.37818(11) 0.85477(7) 0.83109(7) 0.05115(18) Uani 1 1 d . . . . .
Cl1 Cl 0.7529(2) 0.18590(18) 0.46405(8) 0.1295(7) Uani 1 1 d . . . . .
Cl3 Cl -0.16157(14) -0.15412(9) 0.67824(9) 0.0707(3) Uani 1 1 d . . . . .
N3 N 0.3369(3) 0.4949(2) 0.81388(18) 0.0365(4) Uani 1 1 d . . . . .
N4 N 0.5182(3) 0.4931(2) 0.85461(19) 0.0410(5) Uani 1 1 d . . . . .
H4 H 0.594374 0.424784 0.870544 0.049 Uiso 1 1 calc R U . . .
N1 N 0.3427(3) 0.2985(2) 0.64307(16) 0.0359(5) Uani 1 1 d . . . . .
N2 N 0.2970(4) 0.3656(3) 0.54227(19) 0.0444(6) Uani 1 1 d . . . . .
N5 N 0.0123(3) 0.1415(2) 0.78271(18) 0.0364(5) Uani 1 1 d . . . . .
N6 N -0.0959(3) 0.0831(2) 0.8685(2) 0.0452(5) Uani 1 1 d . . . . .
H6 H -0.113189 0.111255 0.928402 0.054 Uiso 1 1 calc R U . . .
C4 C 0.2682(4) 0.6170(2) 0.8013(2) 0.0373(5) Uani 1 1 d . . . . .
H4A H 0.145015 0.647409 0.774962 0.045 Uiso 1 1 calc R U . . .
C5 C 0.4072(4) 0.6923(2) 0.8331(2) 0.0362(5) Uani 1 1 d . . . . .
C6 C 0.5645(4) 0.6104(3) 0.8671(2) 0.0428(6) Uani 1 1 d . . . . .
H6A H 0.681291 0.632208 0.893709 0.051 Uiso 1 1 calc R U . . .
C3 C 0.4229(4) 0.3397(3) 0.4669(2) 0.0520(7) Uani 1 1 d . . . . .
H3 H 0.419802 0.374706 0.392134 0.062 Uiso 1 1 calc R U . . .
C2 C 0.5562(5) 0.2522(4) 0.5209(2) 0.0585(9) Uani 1 1 d . . . . .
C1 C 0.5011(4) 0.2279(3) 0.6302(2) 0.0540(8) Uani 1 1 d . . . . .
H1 H 0.566349 0.170296 0.686125 0.065 Uiso 1 1 calc R U . . .
C7 C 0.0053(4) 0.0696(3) 0.7092(2) 0.0424(6) Uani 1 1 d . . . . .
H7 H 0.067206 0.086035 0.641390 0.051 Uiso 1 1 calc R U . . .
C8 C -0.1086(4) -0.0357(3) 0.7469(2) 0.0414(6) Uani 1 1 d . . . . .
C9 C -0.1713(4) -0.0222(3) 0.8483(3) 0.0482(7) Uani 1 1 d . . . . .
H9 H -0.251756 -0.076806 0.894591 0.058 Uiso 1 1 calc R U . . .
H2 H 0.206(5) 0.412(3) 0.537(3) 0.058(10) Uiso 1 1 d . . . . .
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'
In In -0.7276 1.3100 '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
_geom_angle_publ_flag
Cl6 In1 Cl5 95.88(3) . . ?
Cl6 In1 Cl4 170.94(2) . . ?
Cl5 In1 Cl4 93.07(3) . . ?
N3 In1 Cl6 87.93(6) . . ?
N3 In1 Cl5 93.50(6) . . ?
N3 In1 Cl4 90.13(6) . . ?
N3 In1 N1 90.77(8) . . ?
N3 In1 N5 177.79(8) . . ?
N1 In1 Cl6 86.52(5) . . ?
N1 In1 Cl5 175.17(6) . . ?
N1 In1 Cl4 84.65(5) . . ?
N5 In1 Cl6 90.12(6) . . ?
N5 In1 Cl5 87.74(6) . . ?
N5 In1 Cl4 91.64(6) . . ?
N5 In1 N1 88.07(8) . . ?
N4 N3 In1 126.51(16) . . ?
C4 N3 In1 127.12(17) . . ?
C4 N3 N4 105.6(2) . . ?
N3 N4 H4 124.2 . . ?
C6 N4 N3 111.5(2) . . ?
C6 N4 H4 124.2 . . ?
N2 N1 In1 123.39(16) . . ?
C1 N1 In1 131.23(17) . . ?
C1 N1 N2 105.3(2) . . ?
N1 N2 H2 117(3) . . ?
C3 N2 N1 112.2(2) . . ?
C3 N2 H2 130(3) . . ?
N6 N5 In1 118.87(17) . . ?
C7 N5 In1 135.12(18) . . ?
C7 N5 N6 105.9(2) . . ?
N5 N6 H6 124.3 . . ?
C9 N6 N5 111.4(2) . . ?
C9 N6 H6 124.3 . . ?
N3 C4 H4A 125.0 . . ?
N3 C4 C5 109.9(2) . . ?
C5 C4 H4A 125.0 . . ?
C4 C5 Cl2 125.3(2) . . ?
C6 C5 Cl2 128.5(2) . . ?
C6 C5 C4 106.2(2) . . ?
N4 C6 C5 106.7(2) . . ?
N4 C6 H6A 126.6 . . ?
C5 C6 H6A 126.6 . . ?
N2 C3 H3 127.0 . . ?
N2 C3 C2 106.1(2) . . ?
C2 C3 H3 127.0 . . ?
C3 C2 Cl1 126.1(2) . . ?
C3 C2 C1 106.6(3) . . ?
C1 C2 Cl1 127.4(2) . . ?
N1 C1 C2 109.8(2) . . ?
N1 C1 H1 125.1 . . ?
C2 C1 H1 125.1 . . ?
N5 C7 H7 125.0 . . ?
N5 C7 C8 110.1(2) . . ?
C8 C7 H7 125.0 . . ?
C7 C8 Cl3 126.8(2) . . ?
C9 C8 Cl3 127.5(2) . . ?
C9 C8 C7 105.7(2) . . ?
N6 C9 C8 106.8(2) . . ?
N6 C9 H9 126.6 . . ?
C8 C9 H9 126.6 . . ?
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
In1 Cl6 2.4411(7) . ?
In1 Cl5 2.4547(7) . ?
In1 Cl4 2.4751(7) . ?
In1 N3 2.260(2) . ?
In1 N1 2.303(2) . ?
In1 N5 2.270(2) . ?
Cl2 C5 1.711(3) . ?
Cl1 C2 1.703(3) . ?
Cl3 C8 1.704(3) . ?
N3 N4 1.350(3) . ?
N3 C4 1.330(3) . ?
N4 H4 0.8600 . ?
N4 C6 1.332(4) . ?
N1 N2 1.343(3) . ?
N1 C1 1.315(3) . ?
N2 C3 1.329(4) . ?
N2 H2 0.77(4) . ?
N5 N6 1.358(3) . ?
N5 C7 1.302(4) . ?
N6 H6 0.8600 . ?
N6 C9 1.320(4) . ?
C4 H4A 0.9300 . ?
C4 C5 1.384(4) . ?
C5 C6 1.365(4) . ?
C6 H6A 0.9300 . ?
C3 H3 0.9300 . ?
C3 C2 1.350(4) . ?
C2 C1 1.385(4) . ?
C1 H1 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.395(4) . ?
C8 C9 1.361(4) . ?
C9 H9 0.9300 . ?
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
In1 N3 N4 C6 -171.08(18) . . . . ?
In1 N3 C4 C5 171.23(17) . . . . ?
In1 N1 N2 C3 177.5(2) . . . . ?
In1 N1 C1 C2 -176.9(2) . . . . ?
In1 N5 N6 C9 -177.52(19) . . . . ?
In1 N5 C7 C8 176.15(18) . . . . ?
Cl2 C5 C6 N4 179.2(2) . . . . ?
Cl1 C2 C1 N1 179.2(3) . . . . ?
Cl3 C8 C9 N6 -179.6(2) . . . . ?
N3 N4 C6 C5 0.0(3) . . . . ?
N3 C4 C5 Cl2 -179.48(19) . . . . ?
N3 C4 C5 C6 -0.6(3) . . . . ?
N4 N3 C4 C5 0.6(3) . . . . ?
N1 N2 C3 C2 -0.1(4) . . . . ?
N2 N1 C1 C2 0.7(4) . . . . ?
N2 C3 C2 Cl1 -179.4(3) . . . . ?
N2 C3 C2 C1 0.5(4) . . . . ?
N5 N6 C9 C8 1.1(3) . . . . ?
N5 C7 C8 Cl3 179.1(2) . . . . ?
N5 C7 C8 C9 0.3(3) . . . . ?
N6 N5 C7 C8 0.3(3) . . . . ?
C4 N3 N4 C6 -0.4(3) . . . . ?
C4 C5 C6 N4 0.4(3) . . . . ?
C3 C2 C1 N1 -0.8(5) . . . . ?
C1 N1 N2 C3 -0.4(4) . . . . ?
C7 N5 N6 C9 -0.8(3) . . . . ?
C7 C8 C9 N6 -0.8(3) . . . . ?
