Formation of carbene and cyclopentadienyl ligands from phenylacetylene via oligomerisation and CC bond scission at a mixed-metal W‒Co centre
Davies, John E.; Mays, Martin J.; Raithby, Paul R.; Sarveswaran, Koshala; Solan, Gregory A.; Chemical Communications  (2000) 1313–; doi:10.1039/b003296o

data_7110985
_publ_section_title
;
 Formation of carbene and cyclopentadienyl ligands from phenylacetylene
 via oligomerisation and C&#xE007;C bond scission at a mixed-metal W--Co
 centre
;
_journal_issue                   14
_journal_name_full               'Chemical Communications'
_journal_page_first              1313
_journal_paper_doi               10.1039/b003296o
_journal_year                    2000
_chemical_formula_sum            'C53 H48 Co O4 P W'
_chemical_formula_weight         1022.66
_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                 100.70(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.402(5)
_cell_length_b                   21.565(5)
_cell_length_c                   19.623(5)
_cell_measurement_temperature    180(2)
_cell_volume                     4325(3)
_computing_cell_refinement       'Rigaku control software'
_computing_data_collection       'Rigaku control software'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    'SHELXTL-PLUS (Sheldrick, 1991) '
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.942
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  RAXIS-IIC
_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  0.0780
_diffrn_reflns_av_sigmaI/netI    0.1090
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17678
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    3.125
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7452
_exptl_absorpt_correction_type   'interframe scaling'
_exptl_crystal_colour            'v dark'
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.874
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.821
_refine_ls_shift/su_mean         0.054
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1028
_reflns_number_gt                5765
_reflns_number_total             7611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b003296osup1.cif
_cod_data_source_block           mm9811
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7110985