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_4322944
_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 bis(2,4,6-tri-t-butylbenzene) phosphine (mu-N-methylimidazole)'
_chemical_formula_sum            'C40 H66 N2 P2 Rb2'
_chemical_formula_weight         807.83
_chemical_name_systematic
; 
Rb bis(2,4,6-tri-t-butylbenzene) phosphine (mu-N-methylimidazole) (8)
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.5533(2)
_cell_length_b                   21.4258(5)
_cell_length_c                   28.5990(5)
_cell_measurement_reflns_used    6135
_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.0
_cell_volume                     8917.6(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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            29795
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        <1.0
_diffrn_standards_interval_count n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    2.293
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3392
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.528
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.182
_refine_ls_goodness_of_fit_obs   1.366
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         10027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.236
_refine_ls_restrained_S_obs      1.366
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_obs          0.0461
_refine_ls_shift/esd_max         -0.002
_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         0.1045
_refine_ls_wR_factor_obs         0.0903
_reflns_number_observed          6268
_reflns_number_total             10033
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971178y_6.cif
_cod_data_source_block           rabo
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

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 
;
_cod_database_code               4322944