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_4086939
_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         'C33 H28 Br3 O Os P'
_chemical_formula_sum            'C33 H28 Br3 O Os P'
_chemical_formula_weight         901.45
_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   mixed
_audit_creation_date             2016-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_b                   10.3571(2)
_cell_length_c                   29.9335(7)
_cell_measurement_reflns_used    8865
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      74.8230
_cell_measurement_theta_min      5.1940
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_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega   44.00   88.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -30.0000 44

  2 omega  -49.00   35.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  -90.0000 84

  3 omega   45.00   83.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       40.8203  -99.0000   30.0000 38

  4 omega   41.00  136.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000   60.0000 95

  5 omega   83.00  115.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000   30.0000 32

  6 omega   32.00  142.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -77.0000  -90.0000 110

  7 omega  127.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000 -180.0000 45

  8 omega   57.00  151.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  178.0000  -30.0000 94

  9 omega   90.00  176.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   77.0000   60.0000 86

 10 omega   53.00  124.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000 -180.0000 71

 11 omega   33.00   80.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -90.0000 47

 12 omega   33.00   91.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  120.0000 58

 13 omega  -74.00   25.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   77.0000    0.0000 99

 14 omega -115.00  -11.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000  120.0000 104
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0197216000
_diffrn_orient_matrix_UB_12      -0.1474712000
_diffrn_orient_matrix_UB_13      -0.0029605000
_diffrn_orient_matrix_UB_21      -0.1364713000
_diffrn_orient_matrix_UB_22      0.0190949000
_diffrn_orient_matrix_UB_23      -0.0313106000
_diffrn_orient_matrix_UB_31      0.0770011000
_diffrn_orient_matrix_UB_32      -0.0036039000
_diffrn_orient_matrix_UB_33      -0.0413767000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            16246
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.967
_diffrn_reflns_theta_min         4.522
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    13.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66193
_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
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_exptl_crystal_F_000             1720
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_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         5363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0226
_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^)+(0.0117P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4852
_reflns_number_total             5363
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00860_si_002.cif
_cod_data_source_block           complex10
_cod_depositor_comments
'Adding full bibliography for 4086939--4086941.cif.'
_cod_original_cell_volume        3024.25(12)
_cod_database_code               4086939
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O1(H1A,H1B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), 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)
;
_shelx_res_checksum              26753
_shelx_hkl_checksum              23871
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'