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_4322899
_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 K O P Si2'
_chemical_formula_weight         288.56
_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                   6.4261(2)
_cell_length_b                   12.4119(2)
_cell_length_c                   21.5447(4)
_cell_measurement_reflns_used    5198
_cell_measurement_temperature    150(2)
_cell_volume                     1718.41(7)
_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-96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS-96 (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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            6734
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    0.522
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.115
_exptl_crystal_description       needle
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.07(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         3427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_obs          0.0302
_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^)+(0.0221P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0676
_refine_ls_wR_factor_obs         0.0660
_reflns_number_observed          3104
_reflns_number_total             3427
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9801950_1.cif
_cod_data_source_block           Compound_1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0221P)^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^)+(0.0221P)^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               4322899