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_7711200
_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
'1(C54 H49 Cl6 In6 N12 O8), 3(C5 H12 N), (C3 H6 O)'
_chemical_formula_sum            'C72 H91 Cl6 In6 N15 O9'
_chemical_formula_weight         2154.09
_chemical_name_common
(pipH)3[In6Cl6(\^A?-4-Ph-pz)6(\^A?-OH)6(\^A?3-OH0.5)2]
_chemical_name_systematic        (NC5H12)3[In6Cl6(N2C9H7)6(OH)7O]
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.185(2)
_cell_length_b                   17.185(2)
_cell_length_c                   18.443(2)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.016
_cell_measurement_theta_min      2.370
_cell_volume                     4716.9(9)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45927
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.030
_diffrn_reflns_theta_min         1.758
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0773 before and 0.0438 after correction. The Ratio of minimum to maximum transmission is 0.8441. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.00045(7)
_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   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     171
_refine_ls_number_reflns         2879
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0214P)^2^+9.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0744
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2260
_reflns_number_total             2879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01901a2.cif
_cod_data_source_block           kir055_0m
_cod_original_cell_volume        4717.2(13)
_cod_database_code               7711200
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.607
_olex2_refinement_description
;
1. Restrained distances
 O2-H2A
 1 with sigma of 0.02
2.a Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B), C1AA(H1AA,H1AB)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C6(H6), C5(H5), C7(H7), C8(H8), C9(H9)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              4229
_shelx_hkl_checksum              64033
_shelx_fab_checksum              81669
_olex2_submission_special_instructions 'No special instructions were received'