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_7716988
_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         'H12 I8 Mo6 O6, 4(N O3), 2(H2 O)'
_chemical_formula_sum            'H16 I8 Mo6 N4 O20'
_chemical_formula_weight         1983.01
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2024-06-19 deposited with the CCDC.	2024-09-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.1550(10)
_cell_angle_beta                 90.6780(10)
_cell_angle_gamma                117.1390(10)
_cell_formula_units_Z            2
_cell_length_a                   10.5953(2)
_cell_length_b                   10.7947(2)
_cell_length_c                   15.9552(3)
_cell_measurement_reflns_used    8741
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.46
_cell_volume                     1623.75(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0551
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13976
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.604
_diffrn_reflns_theta_min         1.276
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.056
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: H2O'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.447
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.745
_refine_diff_density_rms         0.291
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         7429
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0333
_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^)+(0.0242P)^2^+2.7418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0817
_refine_ls_wR_factor_ref         0.0836
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6774
_reflns_number_total             7429
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            d4dt01831a2.cif
_cod_data_source_block           juc1406
_cod_depositor_comments
'Adding full bibliography for 7716988--7716991.cif.'
_cod_database_code               7716988
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.199
_shelx_estimated_absorpt_t_max   0.300
_shelx_res_checksum              48096
_shelx_hkl_checksum              79030