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_7711201
_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     'C18 H25 Cl6 In6 N12 O8, 3(C5 H12 N), 1(C3 H6 O)'
_chemical_formula_sum            'C36 H67 Cl6 In6 N15 O9'
_chemical_formula_weight         1755.16
_chemical_name_common            (pipH)3[In6Cl6(?-pz)6(?-OH)6(?3-OH0.5)2]
_chemical_name_systematic        (NC5H12)3[In6Cl6N12C18H25O8]
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-08-17
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-22 deposited with the CCDC.	2022-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                114.005(2)
_cell_angle_beta                 91.512(3)
_cell_angle_gamma                91.947(3)
_cell_formula_units_Z            4
_cell_length_a                   18.801(5)
_cell_length_b                   19.503(5)
_cell_length_c                   20.281(5)
_cell_measurement_reflns_used    9959
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      25.17
_cell_measurement_theta_min      2.17
_cell_volume                     6783(3)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.00
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0654
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            65482
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         25.241
_diffrn_reflns_theta_min         1.884
_exptl_absorpt_coefficient_mu    2.294
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             3422
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1382
_refine_ls_number_reflns         24126
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0182P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16389
_reflns_number_total             24126
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01901a2.cif
_cod_data_source_block           kir057_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C72 H133 Cl12 In12 N30 O18'
_cod_original_formula_weight         3510.32
_cod_original_formula_moiety
'C18 H24 Cl6 In6 N12 O8, C18 H25 Cl6 In6 N12 O8, 6(C5 H12 N), 2(C3 H6 O)'
_cod_original_formula_units_Z            2
_cod_database_code               7711201
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.786
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C12-C5
 1.4 with sigma of 0.02
 C13-C27
 1.4 with sigma of 0.02
 C12-N5
 1.4 with sigma of 0.02
 C6-C19
 1.4 with sigma of 0.02
 N1-C19 = C19-C6
 1.5 with sigma of 0.02
 C19-C6
 1.6 with sigma of 0.02
 C5-C27
 1.6 with sigma of 0.02
 C02A-H02A
 1 with sigma of 0.02
 O0T-H0T
 1 with sigma of 0.02
 O0Y-H0Y
 1 with sigma of 0.02
 O010-H010
 1 with sigma of 0.02
 C028-H028
 1 with sigma of 0.02
 O0W-H0W
 1 with sigma of 0.02
 C4-C3
 1.6 with sigma of 0.02
 C8-C12
 2.52 with sigma of 0.04
 N5-C13
 2.6 with sigma of 0.04
 N5-C5
 2.6 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C8) = Uanis(N5)
4. Rigid body (RIGU) restrains
 N5, H5A, H5B, C8, C12, H8A, H8B, C13, H12A, H12B, C5, H13A, H13B, C27, H5C,
 H5D, H27A, H27B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Secondary CH2 refined with riding coordinates:
 N01L(H01A,H01B), N01U(H01C,H01D), N01V(H01E,H01F), C02L(H1,H), C02R(H02U,
 H02V), C02U(H02L,H02R), C02V(H02X,H02Y), C02Y(H02,HA), C031(H03G,H03H),
 C032(H03I,H03J), C033(H03S,H03T), C034(H03A,H03B), C035(H03K,H03L), N036(H03U,
 H03V), C03A(H03C,H03D), C03B(H03M,H03N), C03D(H03E,H03F), C03H(H03O,H03P),
 C03I(H03Q,H03R), C03J(H03W,H03X), C03K(H03Y,HB), N1(H1A,H1B), C3(H3A,H3B),
 C4(H4A,H4B), C7(H7A,H7B), C19(H19A,H19B), C14(H14A,H14B), C6(H6A,H6B),
 C21(H21A,H21B), C24(H24A,H24B), N5(H5A,H5B), C8(H8A,H8B), C13(H13A,H13B),
 C12(H12A,H12B), C5(H5C,H5D), C27(H27A,H27B)
5.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
5.c Aromatic/amide H refined with riding coordinates:
 O0V(H0V), C01W(H01W), C01Y(H01Y), C01Z(H01Z), C021(H021), C027(H027),
 C029(H029), C02B(H02B), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G),
 C02H(H02H), C02I(H02I), C02J(H02J), C02K(H02K), C02M(H02M), C02N(H02N),
 C02O(H02O), C02P(H02P), C02Q(H02Q), C02S(H02S), C02T(H02T), C02W(H02W),
 C02Z(H02Z), C030(H030), C038(H038)
5.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              4621
_shelx_hkl_checksum              29515
_shelx_fab_checksum              407
_olex2_submission_special_instructions 'No special instructions were received'