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_7009945
_publ_section_title
;
 Synthesis of three-membered metallaphosphaheterocycles and their ring
 opening with Ph2PH on mixed-metal molybdenum--cobalt
 centres&#x200A;&#x2020;
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_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            'C47 H43 Cl2 Co Mo O7 P2'
_chemical_formula_weight         1007.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 102.79(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.676(7)
_cell_length_b                   18.323(4)
_cell_length_c                   12.021(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    180(2)
_cell_volume                     4441(3)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       AFC5R
_diffrn_measurement_method       'omega/2theta scans '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_sigmaI/netI    0.1470
_diffrn_reflns_limit_h_max       999
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -999
_diffrn_reflns_limit_l_max       999
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10808
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0.1%
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'v dark'
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.881
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.014
_refine_ls_goodness_of_fit_obs   1.097
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7822
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.092
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_obs          0.0569
_refine_ls_shift/esd_max         0.111
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+4.5819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1449
_refine_ls_wR_factor_obs         0.1085
_reflns_number_observed          4528
_reflns_number_total             7844
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004594m.txt
_cod_data_source_block           mm9803
_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 2.4.1 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^)+(0.0415P)^2^+4.5819P] 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^)+(0.0415P)^2^+4.5819P] 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        4441.1(28)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009945