A Convenient Synthetic Strategy toward Heavy Alkali Metal Bis(trimethylsilyl)phosphides: Crystal Structures of the Ladder-Type Polymers [A(thf)P(SiMe3)2]∞ (A = K, Rb, Cs)
Ulrich Englich; Karl Hassler; Karin Ruhlandt-Senge; Frank Uhlig; Inorganic Chemistry 37 (1998) 3532–3537; doi:10.1021/ic9801950

data_4322901
_publ_section_title
;
 A Convenient Synthetic Strategy toward Heavy Alkali Metal
 Bis(trimethylsilyl)phosphides: Crystal Structures of the Ladder-Type
 Polymers [A(thf)P(SiMe3)2]\\infty (A = K, Rb, Cs)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3532
_journal_page_last               3537
_journal_paper_doi               10.1021/ic9801950
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C10 H26 Cs O P Si2'
_chemical_formula_weight         382.37
_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                 96.0170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.35150(10)
_cell_length_b                   22.3445(3)
_cell_length_c                   7.25010(10)
_cell_measurement_reflns_used    7544
_cell_measurement_temperature    150(2)
_cell_volume                     1828.81(4)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       '\w for 3 sets, \f for one set of frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            14640
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    2.225
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.9
_refine_diff_density_max         1.188
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.990
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         4342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_obs          0.0481
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1083
_refine_ls_wR_factor_obs         0.0973
_reflns_number_observed          3072
_reflns_number_total             4343
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9801950_3.cif
_cod_data_source_block           Compound_1c
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0528P)^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^)+(0.0528P)^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               4322901