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_7246161
_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         'C68 H52 O7 Os3 P2 Sb2'
_chemical_formula_sum            'C68 H52 O7 Os3 P2 Sb2'
_chemical_formula_weight         1857.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1736(4)
_cell_length_b                   20.3459(6)
_cell_length_c                   21.9689(6)
_cell_measurement_reflns_used    9926
_cell_measurement_temperature    210(1)
_cell_measurement_theta_max      27.18
_cell_measurement_theta_min      2.50
_cell_volume                     6782.3(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0490
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            197248
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.233
_diffrn_reflns_theta_min         2.206
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.482
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1338 before and 0.0708 after correction.
The Ratio of minimum to maximum transmission is 0.4931.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.305
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.979
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.127
_refine_ls_abs_structure_details
;
 Flack x determined using 6318 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0833(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         15130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0265
_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^)+(0.0107P)^2^+30.1444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0603
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                14525
_reflns_number_total             15130
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra07284j2.cif
_cod_data_source_block           fi_1c_a
_cod_database_code               7246161
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.182
_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:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), 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), 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              2132
_shelx_fab_checksum              11215
_olex2_submission_special_instructions 'No special instructions were received'