A new synthetic route for the preparation of [Os3(CO)10(μ-OH)(μ-H)] and its reaction with bis(diphenylphosphino)methane (dppm): syntheses and X-ray structures of two isomers of [Os3(CO)8(μ-OH)(μ-H)(μ-dppm)] and [Os3(CO)7(μ3-CO)(μ3-O)(μ-dppm)]
Joy, Md. Tuhinur R.; Bhoumik, Nikhil C.; Ghosh, Shishir; Richmond, Michael G.; Kabir, Shariff E.; RSC Advances 10 (2020) 44699–44711; doi:10.1039/D0RA08783A

data_7241898
_publ_section_title
;
 A new synthetic route for the preparation of [Os3(CO)10(\m-OH)(\m-H)] and
 its reaction with bis(diphenylphosphino)methane (dppm): syntheses and
 X-ray structures of two isomers of [Os3(CO)8(\m-OH)(\m-H)(\m-dppm)] and
 [Os3(CO)7(\m3-CO)(\m3-O)(\m-dppm)]
;
_journal_issue                   73
_journal_name_full               'RSC Advances'
_journal_page_first              44699
_journal_page_last               44711
_journal_paper_doi               10.1039/D0RA08783A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C33 H22 O9 Os3 P2'
_chemical_formula_sum            'C33 H22 O9 Os3 P2'
_chemical_formula_weight         1195.04
_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     direct
_audit_creation_date             2019-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-11 deposited with the CCDC.	2020-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                63.446(14)
_cell_angle_beta                 81.056(13)
_cell_angle_gamma                68.94(2)
_cell_formula_units_Z            2
_cell_length_a                   12.403(5)
_cell_length_b                   13.586(7)
_cell_length_c                   14.093(6)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.151
_cell_measurement_theta_min      2.869
_cell_volume                     1982.3(16)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53938
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.170
_diffrn_reflns_theta_min         2.904
_exptl_absorpt_coefficient_mu    9.716
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.3925
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1293 before and 0.0675 after correction. The Ratio of minimum to maximum transmission is 0.5265. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.002
_exptl_crystal_description       block
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.111
_refine_diff_density_max         1.866
_refine_diff_density_min         -1.442
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00150(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         8764
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0212
_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^)+(0.0208P)^2^+5.5194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0573
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8352
_reflns_number_total             8764
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra08783a1.cif
_cod_data_source_block           tr_82f
_cod_original_cell_volume        1982.5(16)
_cod_database_code               7241898
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.412
_shelx_estimated_absorpt_t_min   0.183
_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:
 C21(H21a,H21b)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32), C33(H33)
;
_shelx_res_checksum              24268
_shelx_fab_checksum              96456
_olex2_submission_special_instructions 'No special instructions were received'