Electrophilic terminal phosphinidene complex?Lewis base adducts: Chemistry between carbon?halide bond activation and weak Lewis base adduct formation
Ali Khan, Arif; Wismach, Cathleen; Jones, Peter G.; Streubel, Rainer; Chemical Communications  (2003) 2892–; doi:10.1039/b309443j

data_7111305
_publ_section_title
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 Electrophilic terminal phosphinidene complex?Lewis base adducts:
 Chemistry between carbon?halide bond activation and weak Lewis base
 adduct formation
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2892
_journal_paper_doi               10.1039/b309443j
_journal_year                    2003
_chemical_formula_sum            'C19 H26 Br O5 P Si2 W'
_chemical_formula_weight         685.31
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.965(4)
_cell_angle_beta                 88.558(4)
_cell_angle_gamma                68.778(4)
_cell_formula_units_Z            2
_cell_length_a                   9.0099(6)
_cell_length_b                   10.2351(6)
_cell_length_c                   14.4398(11)
_cell_measurement_reflns_used    6756
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.535
_cell_measurement_theta_min      2.588
_cell_volume                     1240.40(15)
_computing_cell_refinement       'Bruker Saint'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SAint'
_computing_molecular_graphics    SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS Smart 1000 CCD'
_diffrn_measurement_method       '\w- & \f-scan'
_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  0.0320
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26263
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    6.454
_exptl_absorpt_correction_T_max  0.8017
_exptl_absorpt_correction_T_min  0.6122
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.350
_refine_diff_density_min         -0.898
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         7239
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0231
_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^)+(0.0247P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0502
_reflns_number_gt                6362
_reflns_number_total             7239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309443jsup1.cif
_cod_data_source_block           gies
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy-atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_database_code               7111305