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_4086940
_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
'C51 H40 Cl4 Os P2, 0.75(C4 H8 O), 0.375(C6 H14)'
_chemical_formula_sum            'C56.25 H51.25 Cl4 O0.75 Os P2'
_chemical_formula_weight         1133.16
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5799(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.91509(14)
_cell_length_b                   17.98521(19)
_cell_length_c                   20.77311(19)
_cell_measurement_reflns_used    21865
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.7090
_cell_measurement_theta_min      3.8330
_cell_volume                     4823.36(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   -8.00   93.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7012   57.0000  120.0000 101

  2 omega  -35.00   52.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7012  -77.0000  -30.0000 87

  3 omega  -56.00   44.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7012  -57.0000 -150.0000 100
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0374733000
_diffrn_orient_matrix_UB_12      -0.0022393000
_diffrn_orient_matrix_UB_13      -0.0255312000
_diffrn_orient_matrix_UB_21      0.0400838000
_diffrn_orient_matrix_UB_22      -0.0048716000
_diffrn_orient_matrix_UB_23      -0.0222841000
_diffrn_orient_matrix_UB_31      -0.0028412000
_diffrn_orient_matrix_UB_32      -0.0390731000
_diffrn_orient_matrix_UB_33      0.0042511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28793
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         3.378
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.972
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2275
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         9417
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0208
_refine_ls_R_factor_gt           0.0181
_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^)+(0.0135P)^2^+6.0261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8754
_reflns_number_total             9417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00860_si_002.cif
_cod_data_source_block           complex11
_cod_depositor_comments
'Adding full bibliography for 4086939--4086941.cif.'
_cod_database_code               4086940
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{O6S, C10S}
3. Restrained distances
 C11S-C12S = C12S-C13S
 1.52 with sigma of 0.02
 C21S-C22S = C23S-C22S
 1.52 with sigma of 0.02
 C5S-C2S
 2.4 with sigma of 0.04
 C3S-O1S
 2.38 with sigma of 0.04
 C4S-O1S
 2.38 with sigma of 0.04
 C5S-C3S
 2.38 with sigma of 0.04
 C4S-C2S
 2.38 with sigma of 0.04
 C4S-C5S \\sim C2S-C3S \\sim C4S-C3S
 with sigma of 0.02
 O1S-C5S \\sim O1S-C2S
 with sigma of 0.02
 C8S-C9S \\sim C8S-C7S
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uiso(O6S) = Uiso(C10S)
5. Others
 Fixed Sof: O1S(0.5) C2S(0.5) C3S(0.5) C4S(0.5) C5S(0.5) O6S(0.25) C7S(0.25)
 C8S(0.25) C9S(0.25) C10S(0.25) C11S(0.25) C12S(0.25) C13S(0.25) C21S(0.5)
 C22S(0.5) C23S(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), 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), C72(H72), C73(H73), C74(H74),
 C75(H75), C76(H76)
;
_shelx_res_checksum              36108
_shelx_hkl_checksum              68349
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-07
_olex2_submission_special_instructions 'No special instructions were received'