Reactions of Osmium Carbyne Complexes OsCl3(≡CR)(PPh3)2 (R = CH═CPh2, CH2Ar) with Bromine and Hydrogen Peroxide
Bai, Wei; Lee, Ka-Ho; Hung, Wai Yiu; Sung, Herman H. Y.; Williams, Ian D.; Lin, Zhenyang; Jia, Guochen; Organometallics 36 (2017) 657–; doi:10.1021/acs.organomet.6b00860

data_4086941
_publ_section_title
;
 Reactions of Osmium Carbyne Complexes OsCl3(\\tb CR)(PPh3)2 (R =
 CH&#x2550;CPh2, CH2Ar) with Bromine and Hydrogen Peroxide
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              657
_journal_paper_doi               10.1021/acs.organomet.6b00860
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C44 H35 Cl3 O Os P2, C4 H10 O'
_chemical_formula_sum            'C48 H45 Cl3 O2 Os P2'
_chemical_formula_weight         1012.33
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.7520(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.36250(10)
_cell_length_b                   18.2899(2)
_cell_length_c                   22.6189(3)
_cell_measurement_reflns_used    17035
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.7490
_cell_measurement_theta_min      9.8870
_cell_volume                     4272.20(8)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  OD_CuKa
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36057
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.997
_diffrn_reflns_theta_min         10.111
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.373
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       block
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.339
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         7513
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0540P)^2^+14.2920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                6919
_reflns_number_total             7513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00860_si_002.cif
_cod_data_source_block           complex13
_cod_depositor_comments
'Adding full bibliography for 4086939--4086941.cif.'
_cod_database_code               4086941
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C5A-C4A = C1A-C2A = C1S-C2S = C4S-C5S
 1.52 with sigma of 0.02
 O3S-C4S \\sim O3A-C4A \\sim O3S-C2S \\sim O3A-C2A
 with sigma of 0.02
3. Others
 Fixed Sof: C1S(0.75) C2S(0.5) O3S(0.6) C4S(0.5) C5S(0.5) C1A(0.25) C2A(0.5)
 O3A(0.4) C4A(0.5) C5A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66)
;
_shelx_res_checksum              68851
_shelx_hkl_checksum              8261
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'