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_4322900
_publ_section_title
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 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 O P Rb Si2'
_chemical_formula_weight         334.93
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   6.5338(2)
_cell_length_b                   12.5664(3)
_cell_length_c                   21.5537(5)
_cell_measurement_reflns_used    5814
_cell_measurement_temperature    150(2)
_cell_volume                     1769.70(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_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
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0834
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11348
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    3.005
_exptl_absorpt_correction_T_max  0.80
_exptl_absorpt_correction_T_min  0.30
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.542
_refine_diff_density_min         -1.445
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.026(11)
_refine_ls_extinction_coef       0.0037(10)
_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   0.975
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         4194
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.980
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_obs          0.0554
_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^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1309
_refine_ls_wR_factor_obs         0.1223
_reflns_number_observed          3197
_reflns_number_total             4195
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9801950_2.cif
_cod_data_source_block           Compound_1b
_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^)+(0.0718P)^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^)+(0.0718P)^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               4322900