Reactions of diphosphine-stabilized Os3 clusters with triphenylantimony: syntheses and structures of new antimony-containing Os3 clusters via Sb–Ph bond cleavage
Islam, Fahmida; Hasan, Md. Sohag; Ghosh, Shishir; Richmond, Michael G.; Kabir, Shariff E.; Roesky, Herbert W.; RSC Advances 13 (2023) 2841–2851; doi:10.1039/D2RA07284J

data_7246160
_publ_section_title
;
 Reactions of diphosphine-stabilized Os3 clusters with triphenylantimony:
 syntheses and structures of new antimony-containing Os3 clusters via
 Sb--Ph bond cleavage
;
_journal_issue                   5
_journal_name_full               'RSC Advances'
_journal_page_first              2841
_journal_page_last               2851
_journal_paper_doi               10.1039/D2RA07284J
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C69 H52 O8 Os3 P2 Sb2'
_chemical_formula_sum            'C69 H52 O8 Os3 P2 Sb2'
_chemical_formula_weight         1885.14
_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_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2022-02-16 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                101.908(2)
_cell_angle_beta                 98.475(2)
_cell_angle_gamma                94.176(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9842(5)
_cell_length_b                   12.2615(4)
_cell_length_c                   22.7266(9)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    193(1)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.44
_cell_volume                     3213.6(2)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      193(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0447
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            74004
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.346
_diffrn_reflns_theta_min         2.229
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.843
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.6690.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       plate
_exptl_crystal_F_000             1780
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.108
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.135
_refine_diff_density_min         -0.902
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     757
_refine_ls_number_reflns         15929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0248P)^2^+6.6432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0589
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12641
_reflns_number_total             15929
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra07284j2.cif
_cod_data_source_block           fi_2c_a
_cod_database_code               7246160
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.781
_shelx_estimated_absorpt_t_min   0.308
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C014(H014), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              17995
_shelx_fab_checksum              32880
_olex2_submission_special_instructions 'No special instructions were received'