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_7711195
_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       '\w 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 \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    1.863
_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+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.161
_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/[\s^2^(Fo^2^)+(0.0098P)^2^+1.1064P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(I)'
_cod_data_source_file            d2dt01901a2.cif
_cod_data_source_block           sh034_01
_cod_database_code               7711195
_shelx_shelxl_version_number     2018/3
_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
_shelx_res_checksum              96556
_shelx_hkl_checksum              46986
_olex2_submission_original_sample_id SH206
_olex2_submission_special_instructions 'No special instructions were received'