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_7246159
_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         'C50 H37 O7 Os3 P2 Sb, C H2 Cl2'
_chemical_formula_sum            'C51 H39 Cl2 O7 Os3 P2 Sb'
_chemical_formula_weight         1589.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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.r6272)
;
_audit_update_record
;
2022-02-16 deposited with the CCDC.	2022-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.6390(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.6929(10)
_cell_length_b                   13.9599(7)
_cell_length_c                   20.1424(10)
_cell_measurement_reflns_used    9241
_cell_measurement_temperature    210(1)
_cell_measurement_theta_max      28.24
_cell_measurement_theta_min      2.69
_cell_volume                     5072.7(4)
_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      210(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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  0.0611
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            115314
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         2.258
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.235
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1055 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.6938.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.081
_exptl_crystal_description       block
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.133
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         12614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0136P)^2^+17.8976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0559
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9804
_reflns_number_total             12614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra07284j2.cif
_cod_data_source_block           fi_1d1_a
_cod_database_code               7246159
_shelx_shelxl_version_number     2014/7
_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:
 C8(H8A,H8B), C51(H51A,H51B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17), C18(H18),
 C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28),
  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)
;
_shelx_res_checksum              25960
_olex2_submission_special_instructions 'No special instructions were received'