μ-1,4-Bis(diphenylphosphino)phenylene-<i>P</i>:<i>P</i>'-bis[μ~3~-benzylidyne-octacarbonyl-<i>triangulo</i>-tricobalt(3 <i>Co</i>—<i>Co</i>)]
Alexander, N. C.; Robinson, B. H.; Simpson, J.; Acta Crystallographica Section C 53 (1997) 425–428; doi:10.1107/S010827019601503X

data_2006058
_publ_contact_author
; Professor Jim Simpson
  Department of Chemistry
  University of Otago
  P.O. Box 56
  Dunedin
  NEW ZEALAND
;
_publ_section_title
;\m-1,4-Bis(diphenylphosphino)phenylene-<i>P</i>:<i>P</i>'-bis[\m~3~-benzylidyne-octacarbonyl-<i>triangulo</i>-tricobalt(3
 <i>Co</i>---<i>Co</i>)]
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              425
_journal_page_last               428
_journal_paper_doi               10.1107/S010827019601503X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac          '[{Co (C O)8 (C7 H5)}2 (C30 H24 P2)]'
_chemical_formula_sum            'C60 H34 Co6 O16 P2'
_chemical_formula_weight         1426.39
_chemical_name_systematic
;\m-1,4-Bis(diphenylphosphino)phenylene-P,P'-bis[\m~3~-benzylidene-octacarbonyl-
triangulo-tricobalt(3
 Co---Co)]
;
_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'
_audit_creation_method           'manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.324(3)
_cell_length_b                   17.688(4)
_cell_length_c                   17.810(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      5
_cell_volume                     2922.4(15)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1992)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_structure_refinement  'SHELX76 (Sheldrick, 1976)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      193(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5127
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.30
_diffrn_standards_decay_%        1.04
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   'empirical \y scans (Sheldrick, 1990)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1428
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.454
_refine_diff_density_min         -0.576
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs
'not available (SHELX76 refinement; Sheldrick, 1976)'
_refine_ls_hydrogen_treatment    'constr (C-H 0.92-0.98\%A) (AFIX SHELX76)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5127
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         0.055
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1.0979/[\s^2^(F) + 0.000241F^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0434
_reflns_number_observed          3369
_reflns_number_total             5127
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1249.cif
_cod_data_source_block           pdum
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w = 1.0979/[\s^2^(F) +
0.000241F^2^]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1.0979/[\s^2^(F) + 0.000241F^2^]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2006058