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_4322939
_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_structural     (Rb(mu-PH(2,4,6-tris-t-butylphenyl))2
_chemical_formula_sum            'C18 H30 P Rb'
_chemical_formula_weight         362.86
_chemical_name_systematic
;
 Rubidium bis(2,4,6-tri-t-butylbenzene)phosphide (3)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                91.3524(13)
_cell_angle_beta                 102.5584(13)
_cell_angle_gamma                107.7966(14)
_cell_formula_units_Z            2
_cell_length_a                   6.71320(10)
_cell_length_b                   10.5022(2)
_cell_length_c                   14.9733(3)
_cell_measurement_reflns_used    3578
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     976.49(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        SAINT
_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      218(2)
_diffrn_measurement_device       'Siemens P4/CCD'
_diffrn_measurement_method       'phi, 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  0.0674
_diffrn_reflns_av_sigmaI/netI    0.1557
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5898
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.40
_diffrn_standards_interval_count NA
_diffrn_standards_interval_time  NA
_diffrn_standards_number         NA
_exptl_absorpt_coefficient_mu    2.608
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.494
_refine_diff_density_rms         0.153
_refine_ls_extinction_coef       0.0097(23)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.891
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         4238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_obs          0.0655
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1914
_refine_ls_wR_factor_obs         0.1466
_reflns_number_observed          2514
_reflns_number_total             4245
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971178y_1.cif
_cod_data_source_block           rabkr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0300P)^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^)+(0.0300P)^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 

2022-02-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C36 H60 P2 Rb2'
_cod_original_formula_weight         725.72
_cod_original_formula_units_Z            1
_cod_original_cell_volume        976.49(4)
_cod_database_code               4322939