Oxo-bridged metal carbene complexes. Synthesis, structure and reactivities of {[Os(Por)(CPh2)]2O} (Por = porphyrinato dianion)
Li, Yan; Huang, Jie-Sheng; Zhou, Zhong-Yuan; Che, Chi-Ming; Chemical Communications (Cambridge, United Kingdom)  (2003) 1362–1363; doi:10.1039/b300441d

data_7113727
_publ_section_title
;
 Oxo-bridged metal carbene complexes. Synthesis, structure and
 reactivities of {[Os(Por)(CPh2)]2O} (Por = porphyrinato dianion)
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   12
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1362
_journal_page_last               1363
_journal_paper_doi               10.1039/b300441d
_journal_year                    2003
_chemical_formula_sum            'C66 H51 N5 Os'
_chemical_formula_weight         1104.32
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 105.290(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.670(5)
_cell_length_b                   11.581(4)
_cell_length_c                   16.707(5)
_cell_measurement_reflns_used    4307
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2737.9(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      294(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.1205
_diffrn_reflns_av_sigmaI/netI    0.1903
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17727
_diffrn_reflns_theta_full        27.63
_diffrn_reflns_theta_max         27.63
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    2.373
_exptl_absorpt_correction_T_max  0.7973
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'SADABS; Sheldrick 1996'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.424
_refine_diff_density_min         -1.684
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         6277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                3061
_reflns_number_total             6277
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103688
_cod_data_source_file            b300441d.txt
_cod_data_source_block           complex_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        2738.0(15)
_cod_original_sg_symbol_H-M      P2/n
_cod_database_code               7113727