Diphosphine Isomerization and C−H and P−C Bond Cleavage Reactivity in the Triosmium Cluster Os3(CO)10(bpcd): Kinetic and Isotope Data for Reversible Ortho Metalation and X-ray Structures of the Bridging and Chelating Isomers of Os3(CO)10(bpcd) and the Benzyne-Substituted Cluster HOs3(CO)8(μ3-C6H4)[μ2,η1-PPhCC(PPh2)C(O)CH2C(O)]†
Watson, William H.; Wu, Guanmin; Richmond, Michael G.; Organometallics 25 (2006) 930–; doi:10.1021/om050839t

data_4074731
_publ_section_title
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 Diphosphine Isomerization and C&#x2212;H and P&#x2212;C Bond Cleavage
 Reactivity in the Triosmium Cluster Os3(CO)10(bpcd):&#x00A0; Kinetic and
 Isotope Data for Reversible Ortho Metalation and X-ray Structures of the
 Bridging and Chelating Isomers of Os3(CO)10(bpcd) and the
 Benzyne-Substituted Cluster
 HOs3(CO)8(\m3-C6H4)[\m2,\h1-PPhCC(PPh2)C(O)CH2C(O)]&#x2020;
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_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              930
_journal_paper_doi               10.1021/om050839t
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C44 H29 O10 Os3 P2'
_chemical_formula_weight         1350.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.281(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.350(6)
_cell_length_b                   11.511(3)
_cell_length_c                   17.383(5)
_cell_measurement_reflns_used    955
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.28
_cell_measurement_theta_min      2.56
_cell_volume                     4167(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2122
_diffrn_reflns_av_sigmaI/netI    0.1581
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            34779
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    9.260
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Red-Brown
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         7.498
_refine_diff_density_min         -2.449
_refine_diff_density_rms         0.400
_refine_ls_extinction_coef       0.00000(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     534
_refine_ls_number_reflns         9724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0780
_refine_ls_shift/su_max          4.092
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1643
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                6477
_reflns_number_total             9724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050839tsi20050929_024137.cif
_cod_data_source_block           w1059m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4074731