Unusual Square Pyramidal Chalcogenide Mo<sub>5</sub> Cluster with Bridging Pyrazolate-Ligands.
Savina, Iulia V.; Ivanov, Anton A.; Evtushok, Darya V.; Gayfulin, Yakov M.; Komarovskikh, Andrey Y.; Syrokvashin, Mikhail M.; Ivanova, Mariia N.; Asanov, Igor P.; Eltsov, Ilia V.; Kuratieva, Natalia V.; Mironov, Yuri V.; Shestopalov, Michael A.; International journal of molecular sciences 24 (2023) 3440–; doi:10.3390/ijms24043440

data_1568597
_publ_section_title
;
 Unusual Square Pyramidal Chalcogenide Mo<sub>5</sub> Cluster with
 Bridging Pyrazolate-Ligands.
;
_journal_issue                   4
_journal_name_full               'International journal of molecular sciences'
_journal_page_first              3440
_journal_paper_doi               10.3390/ijms24043440
_journal_volume                  24
_journal_year                    2023
_chemical_formula_moiety         'C27 H32 Mo5 N18 Se5, 4(C3 H4 N2), Br'
_chemical_formula_sum            'C39 H48 Br Mo5 N26 Se5'
_chemical_formula_weight         1835.44
_space_group_crystal_system      tetragonal
_space_group_IT_number           85
_space_group_name_Hall           '-P 4a'
_space_group_name_H-M_alt        'P 4/n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.6443(4)
_cell_length_b                   15.6443(4)
_cell_length_c                   11.3058(2)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.58
_cell_volume                     2767.03(11)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex DUO 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  0.0251
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.298
_diffrn_reflns_theta_min         1.801
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.203
_exptl_crystal_description       prism
_exptl_crystal_F_000             1758
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.574
_refine_diff_density_max         1.282
_refine_diff_density_min         -1.362
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0197
_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^)+(0.0228P)^2^+3.9618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0493
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3142
_reflns_number_total             3441
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            Mo5red.cif
_cod_data_source_block           jul081_3
_cod_original_cell_volume        2767.03(15)
_cod_original_sg_symbol_H-M      'P 4/n'
_cod_database_code               1568597
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.396
_shelx_estimated_absorpt_t_max   0.576
_shelx_res_checksum              6926
_shelx_hkl_checksum              31641