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_4322946
_publ_contact_author
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        Rabe, Gerd W.
        Technische Universitat Munchen
        Anorganisch-Chemisches Institut
        Lichtenbergstr. 4
        85747 Garching
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_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            'C38 H68 Cs2 N2 P2'
_chemical_formula_weight         880.70
_chemical_name_systematic
;
(10)
;
_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                111.8630(10)
_cell_angle_beta                 100.4120(10)
_cell_angle_gamma                97.4820(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5690(4)
_cell_length_b                   15.0376(5)
_cell_length_c                   15.3643(5)
_cell_measurement_temperature    173(2)
_cell_volume                     2176.13(13)
_computing_cell_refinement       Siemens/SAINT
_computing_data_collection       Siemens/SMART
_computing_data_reduction        Siemens/SAINT
_computing_molecular_graphics    XP-5.03
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-5.03 (Sheldrick, 1994)'
_diffrn_ambient_temperature      173(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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0944
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            13034
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    1.774
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .3
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.326
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.984
_refine_ls_goodness_of_fit_obs   0.993
_refine_ls_hydrogen_treatment    'idealized contributions'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         9349
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.014
_refine_ls_restrained_S_obs      0.993
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_obs          0.0487
_refine_ls_shift/esd_max         0.006
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1702
_refine_ls_wR_factor_obs         0.1408
_reflns_number_observed          6733
_reflns_number_total             9354
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971178y_8.cif
_cod_data_source_block           rabz
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0900P)^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^)+(0.0900P)^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 
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_cod_database_code               4322946