Mononuclear, hexanuclear and polymeric indium(iii) pyrazolido complexes; structural characterization, dynamic solution studies and luminescent properties
Herrera, Susana; Rivero, Kennett I.; Guzmán, Alexis; Cedeño, Jonathan; Miksovska, Jaroslava; Raptis, Raphael G.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01901A

data_7711196
_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       '\w 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 \l/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+0.001xFc^2^\l^3^/sin(2\q)]^-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/[\s^2^(Fo^2^)+(0.0191P)^2^+0.9542P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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
_shelx_res_checksum              31213
_shelx_hkl_checksum              88980
_olex2_submission_original_sample_id SH203
_olex2_submission_special_instructions 'No special instructions were received'