Conversion of a Hydrido‒Butenylcarbyne Complex to η2-Allene-Coordinated Complexes and Metallabenzenes
Chen, Jinxiang; Zhang, Chunhong; Xie, Tingwan; Wen, Ting Bin; Zhang, Hong; Xia, Haiping; Organometallics 32 (2013) 3993–; doi:10.1021/om400469e

data_4081138
_publ_section_title
;
 Conversion of a Hydrido--Butenylcarbyne Complex to \h2-Allene-Coordinated
 Complexes and Metallabenzenes
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              3993
_journal_paper_doi               10.1021/om400469e
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C84 H69 B Cl O Os P3,H6O3'
_chemical_formula_sum            'C84 H75 B Cl O4 Os P3'
_chemical_formula_weight         1477.81
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.322(2)
_cell_angle_beta                 98.837(3)
_cell_angle_gamma                90.171(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5937(5)
_cell_length_b                   15.6767(4)
_cell_length_c                   17.8065(6)
_cell_measurement_reflns_used    4266
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.9190
_cell_measurement_theta_min      3.4020
_cell_volume                     3970.6(2)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'multiwire proportional'
_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  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0802
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29206
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97499
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1508
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.256
_refine_diff_density_min         -0.834
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    conster
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         13975
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0749
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0963P)^2^+6.6993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1783
_reflns_number_gt                11885
_reflns_number_total             13975
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400469e_si_006.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4081138