Octahedral molybdenum iodide clusters with pyrazole or pyrazolate ligands.
Kozlova, Ksenia S.; Berezin, Alexey S.; Kuratieva, Natalia V.; Shestopalov, Michael A.; Ivanov, Anton A.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15959–15967; doi:10.1039/d4dt01831a

data_7716990
_publ_section_title
;
 Octahedral molybdenum iodide clusters with pyrazole or pyrazolate
 ligands.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15959
_journal_page_last               15967
_journal_paper_doi               10.1039/d4dt01831a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H42 I8 K2 Mo6 N24'
_chemical_formula_sum            'C36 H42 I8 K2 Mo6 N24'
_chemical_formula_weight         2479.97
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-03
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
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2024-06-19 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   17.3571(3)
_cell_length_b                   17.3571(3)
_cell_length_c                   17.8314(6)
_cell_measurement_reflns_used    6241
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.35
_cell_volume                     4652.33(19)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      150.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0369
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18111
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.288
_diffrn_reflns_theta_min         2.347
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.343
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0769 before and 0.0508 after correction.
The Ratio of minimum to maximum transmission is 0.8105.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.656
_exptl_crystal_description       block
_exptl_crystal_F_000             3420
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.571
_refine_diff_density_min         -0.532
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.000033(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   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0166P)^2^+7.6749P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0448
_refine_ls_wR_factor_ref         0.0467
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2115
_reflns_number_total             2572
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01831a2.cif
_cod_data_source_block           juc1356c
_cod_depositor_comments
'Adding full bibliography for 7716988--7716991.cif.'
_cod_original_cell_volume        4652.3(2)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7716990
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.856
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Others
 Sof(K1B)=0.33333*(1-FVAR(2))
 Sof(K1A)=0.33333*FVAR(2)
3.a Aromatic/amide H refined with riding coordinates:
 N1S(H1S), C1S(H1SA), C1(H1), C2S(H2S), C2(H2), C3S(H3S), C3(H3)
;
_shelx_res_checksum              80075
_shelx_hkl_checksum              82166
_olex2_submission_special_instructions 'No special instructions were received'