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_4074730
_publ_section_title
;
 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;
;
_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            'C39 H22 O12 Os3 P2'
_chemical_formula_weight         1315.11
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.107(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0279(16)
_cell_length_b                   19.913(3)
_cell_length_c                   18.382(3)
_cell_measurement_reflns_used    1009
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      26.96
_cell_measurement_theta_min      2.84
_cell_volume                     3914.9(10)
_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      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0596
_diffrn_reflns_av_sigmaI/netI    0.0407
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22472
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    9.857
_exptl_absorpt_correction_T_max  0.7019
_exptl_absorpt_correction_T_min  0.1409
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Dark
_exptl_crystal_density_diffrn    2.231
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.298
_refine_diff_density_min         -1.127
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.00045(3)
_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   0.966
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         5120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0619
_reflns_number_gt                4289
_reflns_number_total             5120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om050839tsi20050929_024122.cif
_cod_data_source_block           w999m
_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_cell_volume        3915.0(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4074730