Facile, metal promoted, oxidation of η4-1,3-diphosphacyclobutadiene by water or methanol: synthesis of [MoCl(CO)(η4-1,3-P2C2But2)(η5-L)] (L = C5H5, C5Me5) and [MoCl(CO){η3,λ3,λ5-PC2But2PH(OR)}(η5-L)] (L= C5H5,R = H, Me)
Weller, Andrew S.; Andrews, Christopher D.; Burrows, Andrew D.; Green, Michael; Lynam, Jason M.; Mahon, Mary F.; Jones, Cameron; Chemical Communications  (1999) 2147–; doi:10.1039/a905240b

data_7110642
_publ_section_title
;
 Facile, metal promoted, oxidation of \h4-1,3-diphosphacyclobutadiene by
 water or methanol: synthesis of [MoCl(CO)(\h4-1,3-P2C2But2)(\h5-L)] (L =
 C5H5, C5Me5) and [MoCl(CO){\h3,\l3,\l5-PC2But2PH(OR)}(\h5-L)] (L= C5H5,R
 = H, Me)
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2147
_journal_paper_doi               10.1039/a905240b
_journal_year                    1999
_chemical_formula_sum            'C16.25 H25.5 Cl1.5 Mo O2 P2'
_chemical_formula_weight         463.92
_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                67.90(2)
_cell_angle_beta                 87.66(2)
_cell_angle_gamma                72.600(10)
_cell_formula_units_Z            4
_cell_length_a                   10.067(2)
_cell_length_b                   13.036(4)
_cell_length_c                   17.169(4)
_cell_measurement_temperature    293(2)
_cell_volume                     1985.5(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0097
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7673
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.028
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_F_000             946
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.109
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6971
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.109
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_obs          0.0299
_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^)+(0.0396P)^2^+1.2475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0771
_refine_ls_wR_factor_obs         0.0741
_reflns_number_observed          5817
_reflns_number_total             6974
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            905240bsup1.cif
_cod_data_source_block           compound3
_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 2.4.2 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^)+(0.0396P)^2^+1.2475P] 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^)+(0.0396P)^2^+1.2475P] 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      'P-1 (no.2)'
_cod_original_formula_sum        'C16.25 H25.50 Cl1.50 Mo O2 P2'
_cod_database_code               7110642