Molecular Structures of the Heavier Alkali Metal Salts of Supermesitylphosphane: A Systematic Investigation
Gerd W. Rabe; Henrike Heise; Glenn P. A. Yap; Louise M. Liable-Sands; Ilia A. Guzei; Arnold L. Rheingold; Inorganic Chemistry 37 (1998) 4235–4245; doi:10.1021/ic971178y

data_4322941
_publ_contact_author
;
        Rabe, Gerd W.
        Technische Universitat Munchen
        Anorganisch-Chemisches Institut
        Lichtenbergstr. 4
        85747 Garching
;
_publ_contact_author_email       g.rabe@lrz.tu-muenchen.de
_publ_contact_author_fax         011-49-89-3209-3125
_publ_contact_author_phone       011-49-89-3209-3085
_publ_section_title
;
 Molecular Structures of the Heavier Alkali Metal Salts of
 Supermesitylphosphane: A Systematic Investigation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4235
_journal_page_last               4245
_journal_paper_doi               10.1021/ic971178y
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C46.6 H75.2 Cs2 O0.9 P2'
_chemical_formula_weight         977.63
_chemical_name_systematic
; 
 (5) . toluene 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 91.525(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.039(2)
_cell_length_b                   16.152(3)
_cell_length_c                   20.967(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    243(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      7.5
_cell_volume                     5091.3(17)
_computing_cell_refinement       'Siemens P4'
_computing_data_collection       'Siemens P4'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      243(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       omega
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0838
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7263
_diffrn_reflns_theta_max         21.50
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   'empirical from DIFABS'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.450
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.794
_refine_ls_goodness_of_fit_obs   0.971
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5837
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.836
_refine_ls_restrained_S_obs      0.971
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_obs          0.0501
_refine_ls_shift/esd_max         -0.341
_refine_ls_shift/esd_mean        0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1559
_refine_ls_wR_factor_obs         0.1314
_reflns_number_observed          3230
_reflns_number_total             5850
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971178y_3.cif
_cod_data_source_block           rabj
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] 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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        5091.6(16)
_cod_original_formula_sum        'C46.60 H75.20 Cs2 O0.90 P2'
_cod_database_code               4322941