Generation and Trapping of a Terminal Chlorophosphinidene Complex
Matthew P. Duffy; François Mathey; Journal of the American Chemical Society 131 (2009) 7534–7535; doi:10.1021/ja901918e

data_4104512
_publ_section_title
;
 Generation and Trapping of a Terminal Chlorophosphinidene Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7534
_journal_page_last               7535
_journal_paper_doi               10.1021/ja901918e
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C11 H8 Cl O5 P W'
_chemical_formula_sum            'C11 H8 Cl O5 P W'
_chemical_formula_weight         470.44
_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-97
_cell_angle_alpha                107.800(7)
_cell_angle_beta                 95.428(7)
_cell_angle_gamma                107.102(5)
_cell_formula_units_Z            2
_cell_length_a                   6.6527(7)
_cell_length_b                   10.8920(11)
_cell_length_c                   11.9177(19)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.24
_cell_volume                     769.56(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17156
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    7.792
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.1466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.939
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0210
_refine_ls_R_factor_gt           0.0167
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+0.3615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0394
_refine_ls_wR_factor_ref         0.0428
_reflns_number_gt                3684
_reflns_number_total             4047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja901918e_si_001.cif
_cod_data_source_block           mat5t
_cod_original_cell_volume        769.55(17)
_cod_database_code               4104512