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_1568596
_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, 2(Br), 2(H2 O)'
_chemical_formula_sum            'C27 H36 Br2 Mo5 N18 O2 Se5'
_chemical_formula_weight         1679.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_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            4
_cell_length_a                   15.6320(10)
_cell_length_b                   25.5634(15)
_cell_length_c                   12.2766(8)
_cell_measurement_reflns_used    6489
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.30
_cell_volume                     4905.8(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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20573
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         27.256
_diffrn_reflns_theta_min         2.255
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_description       prism
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.519
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.423(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5450
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0482P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0852
_reflns_Friedel_coverage         0.810
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                4676
_reflns_number_total             5450
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            Mo5ox.cif
_cod_data_source_block           jul086
_cod_database_code               1568596
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.337
_shelx_estimated_absorpt_t_max   0.503
_shelx_res_checksum              6422
_shelx_hkl_checksum              75203