Controllable incorporation of 1,2,4-triazolate into cluster-based metal-chalcogenide frameworks.
Liu, Xiaoshuang; Xue, Chaozhuang; Wang, Xiang; Zhang, Jiaxu; Wu, Tao; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11489–11492; doi:10.1039/d0dt02492a

data_7705025
_publ_section_title
;
 Controllable incorporation of 1,2,4-triazolate into cluster-based
 metal-chalcogenide frameworks.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11489
_journal_page_last               11492
_journal_paper_doi               10.1039/d0dt02492a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C2 H2 In10 N3 S17, 5(C9 H17 N2)'
_chemical_formula_sum            'C47 H87 In10 N13 S17'
_chemical_formula_weight         2527.51
_chemical_name_systematic        SCIF-2
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-09-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-14 deposited with the CCDC.	2020-08-03 downloaded from the CCDC.
;
_cell_angle_alpha                90.00(3)
_cell_angle_beta                 90.00(3)
_cell_angle_gamma                90.00(3)
_cell_formula_units_Z            8
_cell_length_a                   20.887(4)
_cell_length_b                   22.592(5)
_cell_length_c                   33.244(7)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.39
_cell_volume                     15687(6)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0279
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            122997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        23.260
_diffrn_reflns_theta_max         23.260
_diffrn_reflns_theta_min         2.451
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.376
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1803 before and 0.0659 after correction.
The Ratio of minimum to maximum transmission is 0.7494.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_description       block
_exptl_crystal_F_000             9776
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.805
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         11246
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0055P)^2^+55.8658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10300
_reflns_number_total             11246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02492a2.cif
_cod_data_source_block           SCTF-2
_cod_depositor_comments          'Adding full bibliography for 7705025.cif.'
_cod_database_code               7705025
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C014(H01,H), C016(H01A,H01B), C01A(H0AA,HA), C01B(H1AA,HB), C01C(H01M,H01N),
 C01D(H01C,H01D), C01E(H2AA,HC), C01F(H3AA,HD), C01G(H7AA,HE), C01H(H4AA,HF),
 C01K(H8AA,HG), C01L(H01E,H01F), C01M(H01O,H01P), C01N(H5AA,HH), C01O(H01Q,
 H01R), C01P(H01S,H01T), C01Q(H9AA,HI), C01R(H01G,H01H), C01T(H01U,H01V),
 C01U(H01W,H01X), C01V(H01Y,HJ), C01W(H6AA,HK), C01X(H01I,H01J), C01Y(H01Z,HL),
 C01Z(H01K,H01L), C020(H02E,H02F), C021(H02A,H02B), C022(H02G,H02H), C023(H02I,
 H02J), C024(H02K,H02L), C025(H02O,H02P), C026(H02C,H02D), C027(H02M,H02N),
 C028(H02Q,H02R), C029(H02S,H02T), C02A(H02U,H02V), C02C(H02W,H02X), C02D(H02Y,
 HM), C02E(H02Z,HN), C02F(H02,HO)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), N2(H2), N00U(H00U), N00V(H00V), N011(H011), N1I(H1I), C1W(H1W)
;
_shelx_res_checksum              70355
_shelx_fab_checksum              76979
_olex2_submission_special_instructions 'No special instructions were received'