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_4322945
_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            'C39.5 H63.5 Cs2 P2'
_chemical_formula_weight         866.16
_chemical_name_systematic
; 
(9) 
;
_space_group_IT_number           2
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                70.57(3)
_cell_angle_beta                 71.85(3)
_cell_angle_gamma                72.93(2)
_cell_formula_units_Z            2
_cell_length_a                   11.147(4)
_cell_length_b                   14.615(4)
_cell_length_c                   14.806(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2112.4(13)
_computing_cell_refinement       Siemens/XSCANS
_computing_data_collection       Siemens/XSCANS
_computing_data_reduction        Siemens/XSCANS
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXL-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      293(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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0900
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6485
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        <1%
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.825
_exptl_absorpt_correction_T_max  0.586
_exptl_absorpt_correction_T_min  0.450
_exptl_absorpt_correction_type   psi
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       rod
_exptl_crystal_F_000             881
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.864
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.059
_refine_ls_goodness_of_fit_obs   1.148
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         5462
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.148
_refine_ls_R_factor_all          0.1143
_refine_ls_R_factor_obs          0.0513
_refine_ls_shift/esd_max         0.029
_refine_ls_shift/esd_mean        0.001
_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         0.1177
_refine_ls_wR_factor_obs         0.0947
_reflns_number_observed          3175
_reflns_number_total             5462
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971178y_7.cif
_cod_data_source_block           rabv
_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        2112.5(12)
_cod_original_formula_sum        'C39.50 H63.50 Cs2 P2'
_cod_database_code               4322945