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_7009943
_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            'C34 H30 Co Mo O3 P'
_chemical_formula_weight         672.42
_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                 119.27(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.771(19)
_cell_length_b                   28.163(12)
_cell_length_c                   11.014(12)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.5
_cell_volume                     2914(6)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       'Rigaku AFC7R'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -999
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -999
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7863
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.075
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_obs   1.107
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.107
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_obs          0.0701
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+6.9089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2035
_refine_ls_wR_factor_obs         0.1743
_reflns_number_observed          3512
_reflns_number_total             5102
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b004594m.txt
_cod_data_source_block           mm9810
_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^)+(0.1022P)^2^+6.9089P] 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^)+(0.1022P)^2^+6.9089P] 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        2914.5(62)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7009943