#------------------------------------------------------------------------------
#$Date: 2025-08-20 16:06:16 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301830 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/07/43/4074388.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_4074388
loop_
_publ_author_name
'Izod, Keith'
'Wills, Corinne'
'Clegg, William'
'Harrington, Ross W.'
_publ_section_title
;
 Heavier Alkali Metal Complexes of a Silicon- and
 Phosphine-Borane-Stabilized Carbanion
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5326
_journal_paper_doi               10.1021/om0606082
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C18 H50 B Cs N3 P Si2'
_chemical_formula_sum            'C18 H50 B Cs N3 P Si2'
_chemical_formula_weight         539.48
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.165(2)
_cell_angle_beta                 94.135(2)
_cell_angle_gamma                105.163(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0555(12)
_cell_length_b                   11.9069(16)
_cell_length_c                   14.6279(19)
_cell_measurement_reflns_used    9260
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.35
_cell_volume                     1474.5(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10597
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.82
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.399
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.562
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.730
_refine_diff_density_min         -1.892
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.358
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.358
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0490
_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)+(0.0163P)²+2.3833P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                4770
_reflns_number_total             5139
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om0606082si20060705_103118.cif
_cod_data_source_block           11
_cod_database_code               4074388
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cs Cs 0.39776(3) 0.37140(3) 0.31882(2) 0.02687(10) Uani 1 1 d .
B B 0.3846(8) 0.6693(6) 0.5001(4) 0.0382(14) Uani 1 1 d .
H1C H 0.301(6) 0.676(5) 0.551(4) 0.047(15) Uiso 1 1 d .
H1B H 0.407(6) 0.586(5) 0.488(4) 0.053(16) Uiso 1 1 d .
H1A H 0.482(6) 0.740(5) 0.519(4) 0.046(15) Uiso 1 1 d .
N1 N 0.5547(4) 0.2290(4) 0.1694(3) 0.0334(9) Uani 1 1 d .
N2 N 0.2117(4) 0.1552(4) 0.1331(3) 0.0331(9) Uani 1 1 d .
N3 N 0.0880(5) 0.1661(4) 0.3176(3) 0.0356(10) Uani 1 1 d .
P P 0.27803(14) 0.66855(11) 0.38081(8) 0.0285(3) Uani 1 1 d .
Si1 Si 0.58023(15) 0.72712(12) 0.30315(10) 0.0347(3) Uani 1 1 d .
Si2 Si 0.27010(15) 0.64079(12) 0.16633(9) 0.0301(3) Uani 1 1 d .
C1 C 0.3723(5) 0.6510(4) 0.2813(3) 0.0251(10) Uani 1 1 d .
C2 C 0.2063(7) 0.8006(5) 0.3967(4) 0.0453(13) Uani 1 1 d .
H6A H 0.1389 0.7955 0.3395 0.068 Uiso 1 1 calc R
H6B H 0.2938 0.8730 0.4084 0.068 Uiso 1 1 calc R
H6C H 0.1480 0.8041 0.4506 0.068 Uiso 1 1 calc R
C3 C 0.0982(6) 0.5499(5) 0.3693(4) 0.0440(13) Uani 1 1 d .
H5A H 0.0248 0.5543 0.3185 0.066 Uiso 1 1 calc R
H5B H 0.0543 0.5599 0.4288 0.066 Uiso 1 1 calc R
H5C H 0.1190 0.4718 0.3544 0.066 Uiso 1 1 calc R
C4 C 0.0569(6) 0.5677(6) 0.1477(4) 0.0545(16) Uani 1 1 d .
H4A H 0.0367 0.4872 0.1591 0.082 Uiso 1 1 calc R
H4B H 0.0151 0.5619 0.0826 0.082 Uiso 1 1 calc R
H4C H 0.0073 0.6157 0.1915 0.082 Uiso 1 1 calc R
C5 C 0.3434(6) 0.5528(5) 0.0661(4) 0.0438(13) Uani 1 1 d .
H3A H 0.4275 0.6070 0.0445 0.066 Uiso 1 1 calc R
H3B H 0.2593 0.5138 0.0139 0.066 Uiso 1 1 calc R
H3C H 0.3817 0.4918 0.0877 0.066 Uiso 1 1 calc R
C6 C 0.2849(8) 0.7908(5) 0.1390(4) 0.0559(16) Uani 1 1 d .
H2A H 0.3939 0.8358 0.1449 0.084 Uiso 1 1 calc R
H2B H 0.2329 0.8358 0.1834 0.084 Uiso 1 1 calc R
H2C H 0.2355 0.7788 0.0745 0.084 Uiso 1 1 calc R
C7 C 0.6714(7) 0.7367(6) 0.1919(4) 0.0603(17) Uani 1 1 d .
H7A H 0.6657 0.6559 0.1561 0.091 Uiso 1 1 calc R
H7B H 0.7798 0.7844 0.2085 0.091 Uiso 1 1 calc R
H7C H 0.6162 0.7748 0.1534 0.091 Uiso 1 1 calc R
C8 C 0.6322(7) 0.8878(5) 0.3723(4) 0.0497(14) Uani 1 1 d .
H8A H 0.5867 0.9343 0.3366 0.075 Uiso 1 1 calc R
H8B H 0.7448 0.9212 0.3834 0.075 Uiso 1 1 calc R
H8C H 0.5922 0.8913 0.4331 0.075 Uiso 1 1 calc R
C9 C 0.7021(6) 0.6531(5) 0.3666(4) 0.0492(14) Uani 1 1 d .
H9A H 0.7078 0.5794 0.3238 0.074 Uiso 1 1 calc R
H9B H 0.6554 0.6335 0.4217 0.074 Uiso 1 1 calc R
H9C H 0.8063 0.7078 0.3872 0.074 Uiso 1 1 calc R
C10 C 0.7033(6) 0.3115(5) 0.1652(4) 0.0543(16) Uani 1 1 d .
H10A H 0.6865 0.3762 0.1377 0.081 Uiso 1 1 calc R
H10B H 0.7637 0.2684 0.1261 0.081 Uiso 1 1 calc R
H10C H 0.7595 0.3455 0.2291 0.081 Uiso 1 1 calc R
C11 C 0.5769(6) 0.1343(5) 0.2127(4) 0.0498(14) Uani 1 1 d .
H11A H 0.6362 0.1698 0.2757 0.075 Uiso 1 1 calc R
H11B H 0.6334 0.0872 0.1736 0.075 Uiso 1 1 calc R
H11C H 0.4762 0.0820 0.2182 0.075 Uiso 1 1 calc R
C12 C 0.4678(6) 0.1819(5) 0.0747(3) 0.0424(13) Uani 1 1 d .
H12A H 0.5264 0.1369 0.0342 0.051 Uiso 1 1 calc R
H12B H 0.4594 0.2500 0.0479 0.051 Uiso 1 1 calc R
C13 C 0.3062(6) 0.1000(5) 0.0712(3) 0.0370(12) Uani 1 1 d .
H13A H 0.2536 0.0764 0.0055 0.044 Uiso 1 1 calc R
H13B H 0.3147 0.0263 0.0896 0.044 Uiso 1 1 calc R
C14 C 0.1567(7) 0.2396(5) 0.0925(5) 0.0570(16) Uani 1 1 d .
H14A H 0.1062 0.2837 0.1385 0.085 Uiso 1 1 calc R
H14B H 0.0826 0.1965 0.0359 0.085 Uiso 1 1 calc R
H14C H 0.2441 0.2961 0.0754 0.085 Uiso 1 1 calc R
C15 C 0.0830(6) 0.0623(5) 0.1509(4) 0.0427(13) Uani 1 1 d .
H15A H 0.1240 -0.0009 0.1680 0.051 Uiso 1 1 calc R
H15B H 0.0111 0.0254 0.0915 0.051 Uiso 1 1 calc R
C16 C -0.0058(6) 0.1036(5) 0.2262(4) 0.0485(14) Uani 1 1 d .
H16A H -0.0596 0.1580 0.2050 0.058 Uiso 1 1 calc R
H16B H -0.0856 0.0333 0.2348 0.058 Uiso 1 1 calc R
C17 C -0.0123(7) 0.2151(6) 0.3785(4) 0.0587(16) Uani 1 1 d .
H17A H 0.0469 0.2585 0.4403 0.088 Uiso 1 1 calc R
H17B H -0.0984 0.1496 0.3863 0.088 Uiso 1 1 calc R
H17C H -0.0528 0.2701 0.3497 0.088 Uiso 1 1 calc R
C18 C 0.1541(7) 0.0901(6) 0.3604(5) 0.0617(17) Uani 1 1 d .
H18A H 0.2079 0.1346 0.4234 0.093 Uiso 1 1 calc R
H18B H 0.2275 0.0632 0.3214 0.093 Uiso 1 1 calc R
H18C H 0.0721 0.0204 0.3659 0.093 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'
B B 0.0013 0.0007 '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'
Cs Cs -0.3680 2.1192 '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
B Cs H1B 75.6(10) 2_666
B Cs N1 91.92(13) 2_666
B Cs N2 124.19(13) 2_666
B Cs N3 98.42(14) 2_666
B Cs C1 126.06(13) 2_666
H1B Cs N1 152.5(10) .
H1B Cs N2 151.5(10) .
H1B Cs N3 106.2(10) .
H1B Cs C1 58.6(10) .
N1 Cs N2 54.84(10) .
N1 Cs N3 99.81(10) .
N1 Cs C1 115.32(10) .
N2 Cs N3 54.58(10) .
N2 Cs C1 109.28(10) .
N3 Cs C1 119.38(10) .
Cs B H1C 84(3) 2_666
Cs B H1B 65(3) 2_666
Cs B H1A 72(3) 2_666
Cs B P 168.0(3) 2_666
H1C B H1B 112(4) .
H1C B H1A 112(4) .
H1C B P 105(3) .
H1B B H1A 114(4) .
H1B B P 104(3) .
H1A B P 110(3) .
Cs N1 C10 106.0(3) .
Cs N1 C11 102.6(3) .
Cs N1 C12 115.7(3) .
C10 N1 C11 110.3(4) .
C10 N1 C12 109.6(4) .
C11 N1 C12 112.3(4) .
Cs N2 C13 116.8(3) .
Cs N2 C14 90.7(3) .
Cs N2 C15 116.3(3) .
C13 N2 C14 110.7(4) .
C13 N2 C15 109.8(4) .
C14 N2 C15 111.1(4) .
Cs N3 C16 117.6(3) .
Cs N3 C17 109.9(3) .
Cs N3 C18 98.7(3) .
C16 N3 C17 107.1(4) .
C16 N3 C18 113.0(5) .
C17 N3 C18 110.3(5) .
B P C1 118.3(3) .
B P C2 108.5(3) .
B P C3 102.8(3) .
C1 P C2 112.0(2) .
C1 P C3 112.6(2) .
C2 P C3 100.9(3) .
C1 Si1 C7 113.7(2) .
C1 Si1 C8 114.2(2) .
C1 Si1 C9 115.3(2) .
C7 Si1 C8 103.7(3) .
C7 Si1 C9 102.8(3) .
C8 Si1 C9 105.8(3) .
C1 Si2 C4 116.3(2) .
C1 Si2 C5 112.6(2) .
C1 Si2 C6 113.7(2) .
C4 Si2 C5 104.3(3) .
C4 Si2 C6 103.0(3) .
C5 Si2 C6 105.9(2) .
Cs C1 P 88.53(16) .
Cs C1 Si1 96.90(16) .
Cs C1 Si2 113.98(18) .
P C1 Si1 114.4(2) .
P C1 Si2 119.3(2) .
Si1 C1 Si2 117.2(2) .
P C2 H6A 109.5 .
P C2 H6B 109.5 .
P C2 H6C 109.5 .
H6A C2 H6B 109.5 .
H6A C2 H6C 109.5 .
H6B C2 H6C 109.5 .
P C3 H5A 109.5 .
P C3 H5B 109.5 .
P C3 H5C 109.5 .
H5A C3 H5B 109.5 .
H5A C3 H5C 109.5 .
H5B C3 H5C 109.5 .
Si2 C4 H4A 109.5 .
Si2 C4 H4B 109.5 .
Si2 C4 H4C 109.5 .
H4A C4 H4B 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
Si2 C5 H3A 109.5 .
Si2 C5 H3B 109.5 .
Si2 C5 H3C 109.5 .
H3A C5 H3B 109.5 .
H3A C5 H3C 109.5 .
H3B C5 H3C 109.5 .
Si2 C6 H2A 109.5 .
Si2 C6 H2B 109.5 .
Si2 C6 H2C 109.5 .
H2A C6 H2B 109.5 .
H2A C6 H2C 109.5 .
H2B C6 H2C 109.5 .
Si1 C7 H7A 109.5 .
Si1 C7 H7B 109.5 .
Si1 C7 H7C 109.5 .
H7A C7 H7B 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
Si1 C8 H8A 109.5 .
Si1 C8 H8B 109.5 .
Si1 C8 H8C 109.5 .
H8A C8 H8B 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
Si1 C9 H9A 109.5 .
Si1 C9 H9B 109.5 .
Si1 C9 H9C 109.5 .
H9A C9 H9B 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
N1 C10 H10A 109.5 .
N1 C10 H10B 109.5 .
N1 C10 H10C 109.5 .
H10A C10 H10B 109.5 .
H10A C10 H10C 109.5 .
H10B C10 H10C 109.5 .
N1 C11 H11A 109.5 .
N1 C11 H11B 109.5 .
N1 C11 H11C 109.5 .
H11A C11 H11B 109.5 .
H11A C11 H11C 109.5 .
H11B C11 H11C 109.5 .
N1 C12 H12A 108.7 .
N1 C12 H12B 108.7 .
N1 C12 C13 114.2(4) .
H12A C12 H12B 107.6 .
H12A C12 C13 108.7 .
H12B C12 C13 108.7 .
N2 C13 C12 113.4(4) .
N2 C13 H13A 108.9 .
N2 C13 H13B 108.9 .
C12 C13 H13A 108.9 .
C12 C13 H13B 108.9 .
H13A C13 H13B 107.7 .
N2 C14 H14A 109.5 .
N2 C14 H14B 109.5 .
N2 C14 H14C 109.5 .
H14A C14 H14B 109.5 .
H14A C14 H14C 109.5 .
H14B C14 H14C 109.5 .
N2 C15 H15A 108.4 .
N2 C15 H15B 108.4 .
N2 C15 C16 115.4(4) .
H15A C15 H15B 107.5 .
H15A C15 C16 108.4 .
H15B C15 C16 108.4 .
N3 C16 C15 114.5(4) .
N3 C16 H16A 108.6 .
N3 C16 H16B 108.6 .
C15 C16 H16A 108.6 .
C15 C16 H16B 108.6 .
H16A C16 H16B 107.6 .
N3 C17 H17A 109.5 .
N3 C17 H17B 109.5 .
N3 C17 H17C 109.5 .
H17A C17 H17B 109.5 .
H17A C17 H17C 109.5 .
H17B C17 H17C 109.5 .
N3 C18 H18A 109.5 .
N3 C18 H18B 109.5 .
N3 C18 H18C 109.5 .
H18A C18 H18B 109.5 .
H18A C18 H18C 109.5 .
H18B C18 H18C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cs B 3.380(6) 2_666
Cs H1B 3.14(6) .
Cs N1 3.134(4) .
Cs N2 3.312(4) .
Cs N3 3.199(4) .
Cs C1 3.549(4) .
B Cs 3.380(6) 2_666
B H1C 1.11(5) .
B H1B 1.04(6) .
B H1A 1.02(5) .
B P 1.929(6) .
N1 C10 1.458(6) .
N1 C11 1.455(7) .
N1 C12 1.461(6) .
N2 C13 1.462(6) .
N2 C14 1.443(7) .
N2 C15 1.463(6) .
N3 C16 1.466(6) .
N3 C17 1.461(7) .
N3 C18 1.427(7) .
P C1 1.743(4) .
P C2 1.830(5) .
P C3 1.825(5) .
Si1 C1 1.835(4) .
Si1 C7 1.888(6) .
Si1 C8 1.884(6) .
Si1 C9 1.887(5) .
Si2 C1 1.824(4) .
Si2 C4 1.872(6) .
Si2 C5 1.883(5) .
Si2 C6 1.885(6) .
C2 H6A 0.9800 .
C2 H6B 0.9800 .
C2 H6C 0.9800 .
C3 H5A 0.9800 .
C3 H5B 0.9800 .
C3 H5C 0.9800 .
C4 H4A 0.9800 .
C4 H4B 0.9800 .
C4 H4C 0.9800 .
C5 H3A 0.9800 .
C5 H3B 0.9800 .
C5 H3C 0.9800 .
C6 H2A 0.9800 .
C6 H2B 0.9800 .
C6 H2C 0.9800 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C12 C13 1.522(7) .
C13 H13A 0.9900 .
C13 H13B 0.9900 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15A 0.9900 .
C15 H15B 0.9900 .
C15 C16 1.486(7) .
C16 H16A 0.9900 .
C16 H16B 0.9900 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
C18 H18A 0.9800 .
C18 H18B 0.9800 .
C18 H18C 0.9800 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168332170
