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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/7/71/11/7711195.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_7711195
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 H12 Cl3 In N6'
_chemical_formula_sum            'C9 H12 Cl3 In N6'
_chemical_formula_weight         425.42
_chemical_name_common            mer-[InCl3(pzH)3]
_chemical_name_systematic        InCl3(C3N2H4)3
_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   geom
_audit_creation_date             2022-05-17
_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                90
_cell_angle_beta                 106.311(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6493(8)
_cell_length_b                   14.1766(13)
_cell_length_c                   12.8875(12)
_cell_measurement_reflns_used    9706
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.54
_cell_volume                     1516.6(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40A (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19686
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         2.542
_exptl_absorpt_coefficient_mu    2.082
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0464 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.9447.
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    1.863
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol, dichloromethane'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.00408(17)
_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   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         2675
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0181
_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)+(0.0098P)²+1.1064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0364
_refine_ls_wR_factor_ref         0.0378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2434
_reflns_number_total             2675
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01901a2.cif
_cod_data_source_block           sh034_01
_cod_database_code               7711195
_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   0.836
_shelx_estimated_absorpt_t_min   0.774
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), C1(H1), C2(H2A), C3(H3), C4(H4A), C5(H5), C6(H6A),
 C7(H7), C8(H8), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_original_sample_id SH206
_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
In1 In 0.34227(2) 0.34751(2) 0.67164(2) 0.02851(7) Uani 1 1 d . . . . .
Cl1 Cl 0.44553(7) 0.21085(4) 0.78949(5) 0.03920(15) Uani 1 1 d . . . . .
Cl2 Cl 0.38092(8) 0.27636(5) 0.50722(5) 0.04722(17) Uani 1 1 d . . . . .
Cl3 Cl 0.23323(8) 0.49521(5) 0.57487(5) 0.04620(16) Uani 1 1 d . . . . .
N1 N 0.5922(2) 0.41028(13) 0.72288(15) 0.0324(4) Uani 1 1 d . . . . .
N2 N 0.7129(2) 0.37505(14) 0.80455(16) 0.0373(5) Uani 1 1 d . . . . .
H2 H 0.703663 0.326919 0.842986 0.045 Uiso 1 1 calc R U . . .
N3 N 0.3089(2) 0.42280(13) 0.82191(15) 0.0335(4) Uani 1 1 d . . . . .
N4 N 0.2468(2) 0.50976(13) 0.82023(17) 0.0391(5) Uani 1 1 d . . . . .
H4 H 0.215620 0.544122 0.763159 0.047 Uiso 1 1 calc R U . . .
N5 N 0.0882(2) 0.29420(14) 0.64706(16) 0.0350(5) Uani 1 1 d . . . . .
N6 N -0.0399(2) 0.33301(14) 0.57544(16) 0.0385(5) Uani 1 1 d . . . . .
H6 H -0.033830 0.376477 0.530189 0.046 Uiso 1 1 calc R U . . .
C1 C 0.6546(3) 0.48374(18) 0.6857(2) 0.0427(6) Uani 1 1 d . . . . .
H1 H 0.598943 0.522265 0.629131 0.051 Uiso 1 1 calc R U . . .
C2 C 0.8151(3) 0.4950(2) 0.7436(2) 0.0513(7) Uani 1 1 d . . . . .
H2A H 0.885635 0.541281 0.733437 0.062 Uiso 1 1 calc R U . . .
C3 C 0.8480(3) 0.4247(2) 0.8177(2) 0.0469(7) Uani 1 1 d . . . . .
H3 H 0.946416 0.413139 0.868309 0.056 Uiso 1 1 calc R U . . .
C4 C 0.3409(3) 0.39565(19) 0.9236(2) 0.0483(7) Uani 1 1 d . . . . .
H4A H 0.386166 0.337816 0.949744 0.058 Uiso 1 1 calc R U . . .
C5 C 0.2983(4) 0.4647(2) 0.9860(2) 0.0585(8) Uani 1 1 d . . . . .
H5 H 0.308040 0.462198 1.059706 0.070 Uiso 1 1 calc R U . . .
C6 C 0.2396(3) 0.53619(19) 0.9177(2) 0.0486(7) Uani 1 1 d . . . . .
H6A H 0.201141 0.593475 0.935440 0.058 Uiso 1 1 calc R U . . .
C7 C 0.0268(3) 0.23120(18) 0.7006(2) 0.0439(6) Uani 1 1 d . . . . .
H7 H 0.087234 0.193256 0.756184 0.053 Uiso 1 1 calc R U . . .
C8 C -0.1393(3) 0.22981(19) 0.6625(2) 0.0471(7) Uani 1 1 d . . . . .
H8 H -0.210025 0.191633 0.686148 0.057 Uiso 1 1 calc R U . . .
C9 C -0.1774(3) 0.29559(19) 0.5835(2) 0.0448(6) Uani 1 1 d . . . . .
H9 H -0.280583 0.311772 0.542264 0.054 Uiso 1 1 calc R U . . .
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
Cl1 In1 Cl3 172.39(2) . . ?
Cl2 In1 Cl1 95.46(2) . . ?
Cl2 In1 Cl3 92.15(2) . . ?
N1 In1 Cl1 88.75(5) . . ?
N1 In1 Cl2 93.62(5) . . ?
N1 In1 Cl3 90.69(5) . . ?
N1 In1 N3 84.67(7) . . ?
N1 In1 N5 170.36(7) . . ?
N3 In1 Cl1 87.45(5) . . ?
N3 In1 Cl2 176.60(5) . . ?
N3 In1 Cl3 84.94(5) . . ?
N5 In1 Cl1 89.62(5) . . ?
N5 In1 Cl2 95.99(5) . . ?
N5 In1 Cl3 89.68(5) . . ?
N5 In1 N3 85.76(7) . . ?
N2 N1 In1 123.25(14) . . ?
C1 N1 In1 131.19(17) . . ?
C1 N1 N2 105.6(2) . . ?
N1 N2 H2 124.4 . . ?
C3 N2 N1 111.2(2) . . ?
C3 N2 H2 124.4 . . ?
N4 N3 In1 123.84(15) . . ?
C4 N3 In1 131.34(16) . . ?
C4 N3 N4 104.8(2) . . ?
N3 N4 H4 124.2 . . ?
C6 N4 N3 111.6(2) . . ?
C6 N4 H4 124.2 . . ?
N6 N5 In1 122.72(15) . . ?
C7 N5 In1 131.86(17) . . ?
C7 N5 N6 105.0(2) . . ?
N5 N6 H6 124.3 . . ?
C9 N6 N5 111.4(2) . . ?
C9 N6 H6 124.3 . . ?
N1 C1 H1 124.9 . . ?
N1 C1 C2 110.1(2) . . ?
C2 C1 H1 124.9 . . ?
C1 C2 H2A 127.0 . . ?
C3 C2 C1 105.9(2) . . ?
C3 C2 H2A 127.0 . . ?
N2 C3 C2 107.2(2) . . ?
N2 C3 H3 126.4 . . ?
C2 C3 H3 126.4 . . ?
N3 C4 H4A 124.6 . . ?
N3 C4 C5 110.9(2) . . ?
C5 C4 H4A 124.6 . . ?
C4 C5 H5 127.3 . . ?
C6 C5 C4 105.4(2) . . ?
C6 C5 H5 127.3 . . ?
N4 C6 C5 107.3(2) . . ?
N4 C6 H6A 126.4 . . ?
C5 C6 H6A 126.4 . . ?
N5 C7 H7 124.7 . . ?
N5 C7 C8 110.6(2) . . ?
C8 C7 H7 124.7 . . ?
C7 C8 H8 127.2 . . ?
C9 C8 C7 105.5(2) . . ?
C9 C8 H8 127.2 . . ?
N6 C9 C8 107.4(2) . . ?
N6 C9 H9 126.3 . . ?
C8 C9 H9 126.3 . . ?
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
In1 Cl1 2.4690(6) . ?
In1 Cl2 2.4530(6) . ?
In1 Cl3 2.4836(6) . ?
In1 N1 2.2581(18) . ?
In1 N3 2.2994(19) . ?
In1 N5 2.2603(19) . ?
N1 N2 1.353(3) . ?
N1 C1 1.323(3) . ?
N2 H2 0.8600 . ?
N2 C3 1.333(3) . ?
N3 N4 1.342(3) . ?
N3 C4 1.318(3) . ?
N4 H4 0.8600 . ?
N4 C6 1.329(3) . ?
N5 N6 1.345(3) . ?
N5 C7 1.327(3) . ?
N6 H6 0.8600 . ?
N6 C9 1.333(3) . ?
C1 H1 0.9300 . ?
C1 C2 1.388(4) . ?
C2 H2A 0.9300 . ?
C2 C3 1.355(4) . ?
C3 H3 0.9300 . ?
C4 H4A 0.9300 . ?
C4 C5 1.381(4) . ?
C5 H5 0.9300 . ?
C5 C6 1.345(4) . ?
C6 H6A 0.9300 . ?
C7 H7 0.9300 . ?
C7 C8 1.382(4) . ?
C8 H8 0.9300 . ?
C8 C9 1.352(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 N1 N2 C3 179.58(16) . . . . ?
In1 N1 C1 C2 -179.90(17) . . . . ?
In1 N3 N4 C6 179.46(17) . . . . ?
In1 N3 C4 C5 -179.18(19) . . . . ?
In1 N5 N6 C9 -173.77(16) . . . . ?
In1 N5 C7 C8 173.23(17) . . . . ?
N1 N2 C3 C2 0.6(3) . . . . ?
N1 C1 C2 C3 0.1(3) . . . . ?
N2 N1 C1 C2 0.2(3) . . . . ?
N3 N4 C6 C5 -0.1(3) . . . . ?
N3 C4 C5 C6 -0.6(4) . . . . ?
N4 N3 C4 C5 0.5(3) . . . . ?
N5 N6 C9 C8 -0.2(3) . . . . ?
N5 C7 C8 C9 -0.6(3) . . . . ?
N6 N5 C7 C8 0.4(3) . . . . ?
C1 N1 N2 C3 -0.5(3) . . . . ?
C1 C2 C3 N2 -0.5(3) . . . . ?
C4 N3 N4 C6 -0.2(3) . . . . ?
C4 C5 C6 N4 0.4(4) . . . . ?
C7 N5 N6 C9 -0.1(3) . . . . ?
C7 C8 C9 N6 0.5(3) . . . . ?
