The First Structurally Authenticated Rb−PR3and Cs−PR3Contacts. Synthesis and Crystal Structures of [Rb{(Me3Si)2CP(C6H4-2-CH2NMe2)2}]nand [Cs{(Me3Si)2CP(C6H4-2-CH2NMe2)2}(toluene)]n
Izod, Keith; Clegg, William; Liddle, Stephen T.; Organometallics 20 (2001) 367–; doi:10.1021/om0008732

data_4077239
_publ_section_title
;
 The First Structurally Authenticated Rb&#x2212;PR3and
 Cs&#x2212;PR3Contacts. Synthesis and Crystal Structures of
 [Rb{(Me3Si)2CP(C6H4-2-CH2NMe2)2}]nand
 [Cs{(Me3Si)2CP(C6H4-2-CH2NMe2)2}(toluene)]n
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              367
_journal_paper_doi               10.1021/om0008732
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C32 H50 Cs N2 P Si2'
_chemical_formula_weight         682.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.999(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0291(8)
_cell_length_b                   11.2852(4)
_cell_length_c                   16.6256(6)
_cell_measurement_reflns_used    14843
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.31
_cell_volume                     3661.6(2)
_computing_cell_refinement       'Siemens Saint'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0146
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15459
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.52
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.141
_exptl_absorpt_correction_T_max  0.6609
_exptl_absorpt_correction_T_min  0.5005
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.006(7)
_refine_ls_extinction_coef       0.00076(4)
_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_ref   0.919
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         8181
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0392
_refine_ls_wR_factor_ref         0.0394
_reflns_number_gt                7640
_reflns_number_total             8181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0008732.cif
_cod_data_source_block           ki57
_cod_original_sg_symbol_H-M      Cc
_cod_database_code               4077239