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_7716989
_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         'I8 Mo6 O6 H6, 13(H2 O), 2(K)'
_chemical_formula_sum            'H32 I8 K2 Mo6 O19'
_chemical_formula_weight         2005.29
_chemical_properties_physical    Air-sensitive
_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_primary     dual
_audit_creation_date             2024-06-05
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-19 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.590(2)
_cell_angle_beta                 86.932(2)
_cell_angle_gamma                88.658(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6328(4)
_cell_length_b                   11.7341(5)
_cell_length_c                   15.9020(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    220.00
_cell_measurement_theta_max      31.53
_cell_measurement_theta_min      2.53
_cell_volume                     1793.88(13)
_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      220.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            40283
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.547
_diffrn_reflns_theta_min         2.135
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.207
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.5401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1054 before and 0.0500 after correction.
The Ratio of minimum to maximum transmission is 0.7238.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    3.712
_exptl_crystal_description       plate
_exptl_crystal_F_000             1796
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'layering of acetone on water solution'
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.546
_refine_diff_density_min         -2.540
_refine_diff_density_rms         0.208
_refine_ls_extinction_coef       0.00031(4)
_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   1.036
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         11877
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0280P)^2^+4.0854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0681
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10068
_reflns_number_total             11877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01831a2.cif
_cod_data_source_block           juc1538k
_cod_depositor_comments
'Adding full bibliography for 7716988--7716991.cif.'
_cod_database_code               7716989
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.770
_shelx_estimated_absorpt_t_min   0.565
_olex2_refinement_description
;
;
_shelx_res_checksum              91938
_shelx_hkl_checksum              35156
_olex2_submission_special_instructions 'No special instructions were received'