#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:39:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178661 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077238.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4077238
loop_
_publ_author_name
'Izod, Keith'
'Clegg, William'
'Liddle, Stephen T.'
_publ_section_title
;
 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
;
_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            'C25 H42 N2 P Rb Si2'
_chemical_formula_weight         543.23
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.565(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9751(7)
_cell_length_b                   17.7100(12)
_cell_length_c                   15.9534(11)
_cell_measurement_reflns_used    8185
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.51
_cell_measurement_theta_min      2.30
_cell_volume                     2812.9(3)
_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 0.996
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       'ω 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  0.0529
_diffrn_reflns_av_sigmaI/netI    0.0782
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16946
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.917
_exptl_absorpt_correction_T_max  0.5187
_exptl_absorpt_correction_T_min  0.3946
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         6601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0421
_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/[σ²(Fo²)+(0.0414P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0820
_refine_ls_wR_factor_ref         0.0943
_reflns_number_gt                4415
_reflns_number_total             6601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0008732.cif
_cod_data_source_block           ki56
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4077238
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rb Rb 0.08206(3) 0.171598(17) 0.017938(19) 0.02717(10) Uani 1 1 d .
P P -0.14843(7) 0.12849(4) 0.15372(5) 0.01662(16) Uani 1 1 d .
C1 C -0.1279(3) 0.11087(15) 0.26179(17) 0.0193(6) Uani 1 1 d .
Si1 Si 0.04216(8) 0.11839(5) 0.30967(5) 0.0246(2) Uani 1 1 d .
C2 C 0.1121(3) 0.02999(19) 0.3615(2) 0.0413(9) Uani 1 1 d .
H2A H 0.0607 0.0178 0.4101 0.062 Uiso 1 1 calc R
H2B H 0.2065 0.0381 0.3800 0.062 Uiso 1 1 calc R
H2C H 0.1053 -0.0119 0.3213 0.062 Uiso 1 1 calc R
C3 C 0.0582(4) 0.1944(2) 0.3932(2) 0.0412(9) Uani 1 1 d .
H3A H 0.0352 0.2435 0.3679 0.062 Uiso 1 1 calc R
H3B H 0.1508 0.1957 0.4177 0.062 Uiso 1 1 calc R
H3C H -0.0031 0.1833 0.4373 0.062 Uiso 1 1 calc R
C4 C 0.1728(3) 0.14397(18) 0.2338(2) 0.0309(8) Uani 1 1 d .
H4A H 0.1751 0.1051 0.1902 0.046 Uiso 1 1 calc R
H4B H 0.2611 0.1473 0.2641 0.046 Uiso 1 1 calc R
H4C H 0.1501 0.1928 0.2077 0.046 Uiso 1 1 calc R
Si2 Si -0.26466(9) 0.10799(4) 0.33230(5) 0.02278(19) Uani 1 1 d .
C5 C -0.2146(3) 0.05852(17) 0.43399(19) 0.0330(8) Uani 1 1 d .
H5A H -0.1836 0.0073 0.4221 0.050 Uiso 1 1 calc R
H5B H -0.2921 0.0558 0.4687 0.050 Uiso 1 1 calc R
H5C H -0.1420 0.0867 0.4641 0.050 Uiso 1 1 calc R
C6 C -0.4251(3) 0.05892(18) 0.2941(2) 0.0344(8) Uani 1 1 d .
H6A H -0.4618 0.0833 0.2425 0.052 Uiso 1 1 calc R
H6B H -0.4906 0.0623 0.3373 0.052 Uiso 1 1 calc R
H6C H -0.4063 0.0057 0.2828 0.052 Uiso 1 1 calc R
C7 C -0.3215(4) 0.20425(17) 0.3655(2) 0.0362(8) Uani 1 1 d .
H7A H -0.2467 0.2304 0.3959 0.054 Uiso 1 1 calc R
H7B H -0.3961 0.1989 0.4022 0.054 Uiso 1 1 calc R
H7C H -0.3512 0.2336 0.3157 0.054 Uiso 1 1 calc R
C8 C -0.2820(3) 0.20214(15) 0.14140(17) 0.0180(6) Uani 1 1 d .
C9 C -0.4187(3) 0.18458(16) 0.12679(18) 0.0218(6) Uani 1 1 d .
H9 H -0.4439 0.1335 0.1167 0.026 Uiso 1 1 calc R
C10 C -0.5180(3) 0.23920(17) 0.12654(19) 0.0270(7) Uani 1 1 d .
H10 H -0.6097 0.2253 0.1168 0.032 Uiso 1 1 calc R
C11 C -0.4839(3) 0.31370(17) 0.1405(2) 0.0305(8) Uani 1 1 d .
H11 H -0.5516 0.3514 0.1410 0.037 Uiso 1 1 calc R
C12 C -0.3503(3) 0.33292(16) 0.15375(19) 0.0266(7) Uani 1 1 d .
H12 H -0.3271 0.3844 0.1629 0.032 Uiso 1 1 calc R
C13 C -0.2479(3) 0.27907(16) 0.15415(17) 0.0212(6) Uani 1 1 d .
C14 C -0.1047(3) 0.30535(16) 0.17108(19) 0.0241(7) Uani 1 1 d .
H14A H -0.1059 0.3545 0.2005 0.029 Uiso 1 1 calc R
H14B H -0.0575 0.2688 0.2095 0.029 Uiso 1 1 calc R
N1 N -0.0266(2) 0.31399(13) 0.09596(15) 0.0238(6) Uani 1 1 d .
C15 C 0.1060(3) 0.34472(18) 0.1221(2) 0.0363(8) Uani 1 1 d .
H15A H 0.1603 0.3487 0.0732 0.054 Uiso 1 1 calc R
H15B H 0.1508 0.3111 0.1638 0.054 Uiso 1 1 calc R
H15C H 0.0955 0.3949 0.1468 0.054 Uiso 1 1 calc R
C16 C -0.0923(3) 0.36711(19) 0.0363(2) 0.0358(8) Uani 1 1 d .
H16A H -0.0991 0.4167 0.0631 0.054 Uiso 1 1 calc R
H16B H -0.1824 0.3486 0.0191 0.054 Uiso 1 1 calc R
H16C H -0.0392 0.3716 -0.0131 0.054 Uiso 1 1 calc R
C17 C -0.2360(3) 0.04516(15) 0.10237(17) 0.0176(6) Uani 1 1 d .
C18 C -0.2420(3) -0.02033(15) 0.14995(19) 0.0226(6) Uani 1 1 d .
H18 H -0.2047 -0.0197 0.2062 0.027 Uiso 1 1 calc R
C19 C -0.2999(3) -0.08620(16) 0.1191(2) 0.0253(7) Uani 1 1 d .
H19 H -0.3025 -0.1297 0.1538 0.030 Uiso 1 1 calc R
C20 C -0.3544(3) -0.08855(16) 0.0370(2) 0.0264(7) Uani 1 1 d .
H20 H -0.3979 -0.1328 0.0155 0.032 Uiso 1 1 calc R
C21 C -0.3442(3) -0.02530(17) -0.01288(19) 0.0254(7) Uani 1 1 d .
H21 H -0.3789 -0.0273 -0.0697 0.031 Uiso 1 1 calc R
C22 C -0.2843(3) 0.04161(16) 0.01769(18) 0.0208(6) Uani 1 1 d .
C23 C -0.2765(3) 0.10696(17) -0.04282(18) 0.0236(7) Uani 1 1 d .
H23A H -0.3501 0.1018 -0.0870 0.028 Uiso 1 1 calc R
H23B H -0.2915 0.1545 -0.0121 0.028 Uiso 1 1 calc R
N2 N -0.1479(2) 0.11301(14) -0.08358(15) 0.0265(6) Uani 1 1 d .
C24 C -0.1222(3) 0.0456(2) -0.1322(2) 0.0449(9) Uani 1 1 d .
H24A H -0.1991 0.0360 -0.1721 0.067 Uiso 1 1 calc R
H24B H -0.1091 0.0024 -0.0943 0.067 Uiso 1 1 calc R
H24C H -0.0413 0.0532 -0.1630 0.067 Uiso 1 1 calc R
C25 C -0.1544(4) 0.17826(19) -0.1400(2) 0.0392(8) Uani 1 1 d .
H25A H -0.0694 0.1829 -0.1674 0.059 Uiso 1 1 calc R
H25B H -0.1698 0.2242 -0.1077 0.059 Uiso 1 1 calc R
H25C H -0.2282 0.1714 -0.1828 0.059 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N2 Rb N1 103.56(7) . .
N2 Rb C20 109.28(7) . 3
N1 Rb C20 144.00(7) . 3
N2 Rb P 74.32(5) . .
N1 Rb P 69.35(5) . .
C20 Rb P 133.62(6) 3 .
N2 Rb C7 94.55(8) . 4_665
N1 Rb C7 83.25(7) . 4_665
C20 Rb C7 79.90(8) 3 4_665
P Rb C7 146.42(6) . 4_665
N2 Rb C19 89.82(7) . 3
N1 Rb C19 149.34(7) . 3
C20 Rb C19 23.20(7) 3 3
P Rb C19 141.30(5) . 3
C7 Rb C19 68.10(7) 4_665 3
N2 Rb C21 105.81(7) . 3
N1 Rb C21 149.67(6) . 3
C20 Rb C21 21.85(7) 3 3
P Rb C21 111.78(5) . 3
C7 Rb C21 101.70(7) 4_665 3
C19 Rb C21 38.53(7) 3 3
C1 P C8 105.49(13) . .
C1 P C17 108.19(13) . .
C8 P C17 101.18(12) . .
C1 P Rb 129.46(10) . .
C8 P Rb 106.70(9) . .
C17 P Rb 102.52(9) . .
P C1 Si2 124.53(16) . .
P C1 Si1 116.63(16) . .
Si2 C1 Si1 117.17(15) . .
C1 Si1 C2 115.65(14) . .
C1 Si1 C4 114.25(13) . .
C2 Si1 C4 103.26(15) . .
C1 Si1 C3 112.51(15) . .
C2 Si1 C3 105.60(16) . .
C4 Si1 C3 104.43(15) . .
C1 Si2 C7 113.49(14) . .
C1 Si2 C5 112.10(14) . .
C7 Si2 C5 104.29(15) . .
C1 Si2 C6 117.77(14) . .
C7 Si2 C6 104.09(15) . .
C5 Si2 C6 103.75(15) . .
C9 C8 C13 117.3(2) . .
C9 C8 P 122.8(2) . .
C13 C8 P 119.6(2) . .
C10 C9 C8 122.2(3) . .
C11 C10 C9 119.9(3) . .
C10 C11 C12 119.2(3) . .
C11 C12 C13 122.1(3) . .
C12 C13 C8 119.1(3) . .
C12 C13 C14 118.3(3) . .
C8 C13 C14 122.6(3) . .
N1 C14 C13 115.3(2) . .
C16 N1 C15 107.8(2) . .
C16 N1 C14 110.9(2) . .
C15 N1 C14 108.6(2) . .
C16 N1 Rb 115.05(19) . .
C15 N1 Rb 94.93(17) . .
C14 N1 Rb 117.73(16) . .
C18 C17 C22 117.6(3) . .
C18 C17 P 116.9(2) . .
C22 C17 P 125.2(2) . .
C19 C18 C17 122.9(3) . .
C18 C19 C20 119.6(3) . .
C18 C19 Rb 108.93(19) . 3
C20 C19 Rb 67.75(16) . 3
C21 C20 C19 118.8(3) . .
C21 C20 Rb 96.81(18) . 3
C19 C20 Rb 89.05(17) . 3
C20 C21 C22 122.0(3) . .
C20 C21 Rb 61.33(16) . 3
C22 C21 Rb 108.32(17) . 3
C21 C22 C17 119.0(3) . .
C21 C22 C23 117.6(3) . .
C17 C22 C23 123.4(2) . .
N2 C23 C22 114.7(2) . .
C24 N2 C25 108.8(3) . .
C24 N2 C23 111.2(2) . .
C25 N2 C23 108.8(2) . .
C24 N2 Rb 115.47(19) . .
C25 N2 Rb 93.67(18) . .
C23 N2 Rb 117.12(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb N2 2.915(2) .
Rb N1 3.042(2) .
Rb C20 3.257(3) 3
Rb P 3.3437(8) .
Rb C7 3.459(3) 4_665
Rb C19 3.519(3) 3
Rb C21 3.686(3) 3
P C1 1.752(3) .
P C8 1.866(3) .
P C17 1.877(3) .
C1 Si2 1.822(3) .
C1 Si1 1.822(3) .
Si1 C2 1.884(3) .
Si1 C4 1.888(3) .
Si1 C3 1.894(3) .
Si2 C7 1.883(3) .
Si2 C5 1.884(3) .
Si2 C6 1.889(3) .
C8 C9 1.404(4) .
C8 C13 1.416(4) .
C9 C10 1.385(4) .
C10 C11 1.377(4) .
C11 C12 1.379(4) .
C12 C13 1.397(4) .
C13 C14 1.511(4) .
C14 N1 1.477(4) .
N1 C16 1.463(4) .
N1 C15 1.466(4) .
C17 C18 1.389(4) .
C17 C22 1.407(4) .
C18 C19 1.379(4) .
C19 C20 1.386(4) .
C19 Rb 3.519(3) 3
C20 C21 1.382(4) .
C20 Rb 3.257(3) 3
C21 C22 1.401(4) .
C21 Rb 3.686(3) 3
C22 C23 1.512(4) .
C23 N2 1.478(4) .
N2 C24 1.454(4) .
N2 C25 1.464(4) .
