Formation of a Novel P,C-Cage Ligand via aP-C5Me5-Substituted Li/Cl Phosphinidenoid Complex
Bode, Maren; Daniels, Jörg; Streubel, Rainer; Organometallics 28 (2009) 4636–; doi:10.1021/om900331g

data_4069639
_publ_section_title
;
 Formation of a Novel P,C-Cage Ligand via aP-C5Me5-Substituted Li/Cl
 Phosphinidenoid Complex
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              4636
_journal_paper_doi               10.1021/om900331g
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C30 H30 O10 P2 W2'
_chemical_formula_weight         980.18
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-07-04T10:50:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 93.5930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9232(3)
_cell_length_b                   14.0356(4)
_cell_length_c                   19.5914(3)
_cell_measurement_reflns_used    21562
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3272.16(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.208846E-1
_diffrn_orient_matrix_UB_12      -0.657034E-1
_diffrn_orient_matrix_UB_13      -0.143339E-1
_diffrn_orient_matrix_UB_21      0.425541E-1
_diffrn_orient_matrix_UB_22      0.274005E-1
_diffrn_orient_matrix_UB_23      -0.377719E-1
_diffrn_orient_matrix_UB_31      0.693915E-1
_diffrn_orient_matrix_UB_32      0.29713E-2
_diffrn_orient_matrix_UB_33      0.313612E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30441
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.9
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    7.177
_exptl_absorpt_correction_T_max  0.4658
_exptl_absorpt_correction_T_min  0.2709
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        (see. N.W. Alcock (1970). Cryst. Computing, p271)
;
_exptl_crystal_colour            paleyellow
_exptl_crystal_density_diffrn    1.99
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.802
_refine_diff_density_min         -1.552
_refine_diff_density_rms         0.168
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.045
_reflns_number_gt                6532
_reflns_number_total             7395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900331g_si_002.cif
_cod_data_source_block           joerg158
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4069639