Alkyne‒phosphinoalkyne coupling reactions on mixed-metal tungsten‒cobalt centres; P‒C(alkyne) bond cleavage versus P‒C(alkyne) bond preservation
Davies, John E.; Mays, Martin J.; Raithby, Paul R.; Sarveswaran, Koshala; Solan, Gregory A.; Journal of the Chemical Society, Dalton Transactions  (2001) 1269–; doi:10.1039/b009396n

data_7010468
_publ_section_title
;
 Alkyne--phosphinoalkyne coupling reactions on mixed-metal
 tungsten--cobalt centres; P--C(alkyne) bond cleavage versus
 P--C(alkyne) bond preservation
;
_journal_issue                   8
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1269
_journal_paper_doi               10.1039/b009396n
_journal_year                    2001
_chemical_formula_sum            'C39 H30 Co Fe O8 P W'
_chemical_formula_weight         956.23
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 103.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.688(6)
_cell_length_b                   17.919(9)
_cell_length_c                   17.359(9)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     3535(3)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'Stoe diffractometer'
_diffrn_measurement_method       'omega-theta 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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4644
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.52
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.214
_exptl_absorpt_correction_T_max  0.361
_exptl_absorpt_correction_T_min  0.285
_exptl_absorpt_correction_type   'semi-empirical psi scans'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_description       block
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.122
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_hydrogen_treatment    'Riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         4594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.154
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.0404
_refine_ls_R_factor_obs          0.0308
_refine_ls_shift/esd_max         0.015
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+11.6976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0864
_refine_ls_wR_factor_obs         0.0780
_reflns_number_observed          4011
_reflns_number_total             4605
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b009396n.txt
_cod_data_source_block           mm9806
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0360P)^2^+11.6976P] 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^)+(0.0360P)^2^+11.6976P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3534.6(31)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010468