Synthesis of three-membered metallaphosphaheterocycles and their ring opening with Ph2PH on mixed-metal molybdenum‒cobalt centres †
Davies, John E.; Mays, Martin J.; Raithby, Paul R.; Sarveswaran, Koshala; Solan, Gregory A.; Journal of the Chemical Society, Dalton Transactions  (2000) 3331–; doi:10.1039/b004594m

data_7009946
_publ_section_title
;
 Synthesis of three-membered metallaphosphaheterocycles and their ring
 opening with Ph2PH on mixed-metal molybdenum--cobalt
 centres&#x200A;&#x2020;
;
_journal_issue                   19
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3331
_journal_paper_doi               10.1039/b004594m
_journal_year                    2000
_chemical_formula_sum            'C33.5 H37.5 Cl Co0.5 Mo0.5 O P1.5'
_chemical_formula_weight         615.48
_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
_cell_angle_alpha                103.78(3)
_cell_angle_beta                 91.12(3)
_cell_angle_gamma                76.21(3)
_cell_formula_units_Z            4
_cell_length_a                   15.460(5)
_cell_length_b                   18.534(5)
_cell_length_c                   11.506(5)
_cell_measurement_temperature    180(2)
_cell_volume                     3107(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       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  0.1227
_diffrn_reflns_av_sigmaI/netI    0.2132
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19369
_diffrn_reflns_theta_max         25.18
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    0.674
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             1282
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.572
_refine_diff_density_min         -1.633
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.032
_refine_ls_goodness_of_fit_obs   1.338
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         10482
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.086
_refine_ls_restrained_S_obs      1.345
_refine_ls_R_factor_all          0.1962
_refine_ls_R_factor_obs          0.1044
_refine_ls_shift/esd_max         -10.615
_refine_ls_shift/esd_mean        0.164
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1737P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3402
_refine_ls_wR_factor_obs         0.2871
_reflns_number_observed          4972
_reflns_number_total             10516
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004594m.txt
_cod_data_source_block           mm9809
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1737P)^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^)+(0.1737P)^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_cell_volume        3107.3(19)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C33.50 H37.50 Cl Co0.50 Mo0.50 O P1.50'
_cod_database_code               7009946