2,5-Diphenyl-3,4-bis(trimethylsilyl)-1-phosphacyclopentadienide as a Ligand at Calcium, Strontium, and Tin(II)
Matthias Westerhausen; Matthias H. Digeser; Heinrich Nöth; Werner Ponikwar; Thomas Seifert; Kurt Polborn; Inorganic Chemistry 38 (1999) 3207–3214; doi:10.1021/ic981132k

data_4322095
_publ_contact_author
;
    Matthias Westerhausen
    Institut fuer Anorganische Chemie
    Ludwig-Maximilians-Universitaet Muenchen
    Meiserstr. 1
    D-80333 Muenchen
    Germany
;
_publ_contact_author_email       maw@anorg.chemie.uni-muenchen.de
_publ_contact_author_fax         '+49 (89) 5902 578'
_publ_contact_author_phone       '+49 (89) 5902 638'
_publ_section_title
;
 2,5-Diphenyl-3,4-bis(trimethylsilyl)-1-phosphacyclopentadienide as a
 Ligand at Calcium, Strontium, and Tin(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3207
_journal_page_last               3214
_journal_paper_doi               10.1021/ic981132k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C74 H104 Ca O4 P2 Si4'
_chemical_formula_weight         1271.95
_chemical_melting_point          311(2)
_chemical_name_systematic
; 
 tetrakis(thf)calcium 
 bis(2,5-diphenyl-3,4-bis(trimethylsilyl)phosphacyclopentadienide 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.000(12)
_cell_angle_beta                 93.365(10)
_cell_angle_gamma                90.000(12)
_cell_formula_units_Z            4
_cell_length_a                   21.089(3)
_cell_length_b                   12.962(2)
_cell_length_c                   27.353(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      16
_cell_measurement_theta_min      9
_cell_volume                     7464.2(18)
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       Nonius_CAD4_Mach3
_diffrn_measurement_method       omega-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  0.0087
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4523
_diffrn_reflns_theta_max         21.67
_diffrn_reflns_theta_min         2.34
_diffrn_standards_decay_%        -34.2
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .30
_exptl_crystal_size_min          .20
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.075
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_obs          0.0521
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+17.8046P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1381
_refine_ls_wR_factor_obs         0.1227
_reflns_number_observed          3347
_reflns_number_total             4377
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic981132k_1.cif
_cod_data_source_block           capc4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+17.8046P] 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^)+(0.0568P)^2^+17.8046P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322095