#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:36:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179979 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/73/7027307.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027307
loop_
_publ_author_name
'Clegg, William'
'Doherty, Simon'
'Izod, Keith'
'Kagerer, Hartmut'
'O’Shaughnessy, Paul'
'Sheffield, Joanne M.'
_publ_section_title
;
 Monomeric alkali metal complexes of a sterically demanding,
 donor-functionalised secondary phosphide ligand
;
_journal_issue                   11
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1825
_journal_paper_doi               10.1039/a900869a
_journal_year                    1999
_chemical_formula_sum            'C25 H54 K N4 P Si2'
_chemical_formula_weight         536.97
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.877(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1740(2)
_cell_length_b                   28.7226(6)
_cell_length_c                   12.1761(3)
_cell_measurement_reflns_used    10470
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.64
_cell_measurement_theta_min      2.27
_cell_volume                     3366.77(13)
_computing_cell_refinement       'local programs'
_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 0.903
_diffrn_measured_fraction_theta_max 0.903
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21064
_diffrn_reflns_theta_full        28.82
_diffrn_reflns_theta_max         28.82
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.907
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         7949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0815
_refine_ls_R_factor_gt           0.0447
_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)+(0.0485P)²+0.2726P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                5451
_reflns_number_total             7949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900869asup1.cif
_cod_data_source_block           compound_4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7027307
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
K K 0.11439(4) 0.138678(15) 0.96175(4) 0.02908(11) Uani 1 1 d .
P P -0.20488(5) 0.112212(17) 0.82186(4) 0.02660(12) Uani 1 1 d .
N1 N -0.01061(15) 0.12928(5) 1.13449(13) 0.0273(4) Uani 1 1 d .
N2 N 0.27129(17) 0.05441(6) 0.99292(16) 0.0384(4) Uani 1 1 d .
N3 N 0.40898(15) 0.14564(5) 1.06614(13) 0.0274(4) Uani 1 1 d .
N4 N 0.24293(16) 0.22791(6) 0.96456(14) 0.0317(4) Uani 1 1 d .
Si1 Si -0.17290(6) 0.08401(2) 0.58869(5) 0.03265(14) Uani 1 1 d .
Si2 Si -0.47478(5) 0.09981(2) 0.62282(4) 0.02925(14) Uani 1 1 d .
C1 C -0.28728(19) 0.11545(7) 0.65728(15) 0.0270(4) Uani 1 1 d .
H1A H -0.2851 0.1490 0.6360 0.032 Uiso 1 1 calc R
C2 C -0.1338(3) 0.02345(8) 0.6454(2) 0.0488(6) Uani 1 1 d .
H2A H -0.0993 0.0241 0.7304 0.073 Uiso 1 1 calc R
H2B H -0.0631 0.0098 0.6165 0.073 Uiso 1 1 calc R
H2C H -0.2187 0.0046 0.6191 0.073 Uiso 1 1 calc R
C3 C -0.0062(2) 0.11683(9) 0.6156(2) 0.0511(6) Uani 1 1 d .
H3A H -0.0258 0.1475 0.5784 0.077 Uiso 1 1 calc R
H3B H 0.0554 0.0994 0.5832 0.077 Uiso 1 1 calc R
H3C H 0.0390 0.1208 0.6993 0.077 Uiso 1 1 calc R
C4 C -0.2513(2) 0.07992(10) 0.42649(19) 0.0521(6) Uani 1 1 d .
H4A H -0.3351 0.0606 0.4067 0.078 Uiso 1 1 calc R
H4B H -0.1840 0.0658 0.3942 0.078 Uiso 1 1 calc R
H4C H -0.2756 0.1112 0.3940 0.078 Uiso 1 1 calc R
C5 C -0.5608(2) 0.13985(8) 0.70024(18) 0.0381(5) Uani 1 1 d .
H5A H -0.5141 0.1375 0.7842 0.057 Uiso 1 1 calc R
H5B H -0.6587 0.1311 0.6820 0.057 Uiso 1 1 calc R
H5C H -0.5547 0.1720 0.6751 0.057 Uiso 1 1 calc R
C6 C -0.5772(2) 0.10642(10) 0.46424(18) 0.0522(7) Uani 1 1 d .
H6A H -0.5619 0.1376 0.4379 0.078 Uiso 1 1 calc R
H6B H -0.6763 0.1022 0.4530 0.078 Uiso 1 1 calc R
H6C H -0.5468 0.0829 0.4193 0.078 Uiso 1 1 calc R
C7 C -0.4967(2) 0.03838(8) 0.6640(2) 0.0467(6) Uani 1 1 d .
H7A H -0.4617 0.0171 0.6169 0.070 Uiso 1 1 calc R
H7B H -0.5954 0.0321 0.6505 0.070 Uiso 1 1 calc R
H7C H -0.4445 0.0336 0.7463 0.070 Uiso 1 1 calc R
C8 C -0.21259(17) 0.17143(6) 0.87090(15) 0.0236(4) Uani 1 1 d .
C9 C -0.2452(2) 0.21141(7) 0.79826(17) 0.0316(4) Uani 1 1 d .
H9A H -0.2633 0.2074 0.7172 0.038 Uiso 1 1 calc R
C10 C -0.2519(2) 0.25563(7) 0.83985(18) 0.0364(5) Uani 1 1 d .
H10A H -0.2739 0.2811 0.7873 0.044 Uiso 1 1 calc R
C11 C -0.2269(2) 0.26348(7) 0.95684(19) 0.0361(5) Uani 1 1 d .
H11A H -0.2319 0.2939 0.9856 0.043 Uiso 1 1 calc R
C12 C -0.19441(19) 0.22547(7) 1.03088(18) 0.0307(4) Uani 1 1 d .
H12A H -0.1775 0.2304 1.1114 0.037 Uiso 1 1 calc R
C13 C -0.18552(17) 0.18037(6) 0.99225(16) 0.0244(4) Uani 1 1 d .
C14 C -0.15855(18) 0.14090(7) 1.07796(16) 0.0272(4) Uani 1 1 d .
H14A H -0.1997 0.1490 1.1389 0.033 Uiso 1 1 calc R
H14B H -0.2071 0.1128 1.0374 0.033 Uiso 1 1 calc R
C15 C 0.0571(2) 0.16501(8) 1.21911(19) 0.0429(5) Uani 1 1 d .
H15A H 0.0080 0.1682 1.2760 0.064 Uiso 1 1 calc R
H15B H 0.0549 0.1948 1.1792 0.064 Uiso 1 1 calc R
H15C H 0.1537 0.1560 1.2590 0.064 Uiso 1 1 calc R
C16 C 0.0007(2) 0.08472(8) 1.1938(2) 0.0451(6) Uani 1 1 d .
H16A H 0.0989 0.0769 1.2306 0.068 Uiso 1 1 calc R
H16B H -0.0443 0.0605 1.1375 0.068 Uiso 1 1 calc R
H16C H -0.0449 0.0868 1.2533 0.068 Uiso 1 1 calc R
C17 C 0.2045(3) 0.01483(9) 1.0290(3) 0.0638(8) Uani 1 1 d .
H17A H 0.1071 0.0130 0.9797 0.096 Uiso 1 1 calc R
H17B H 0.2093 0.0189 1.1101 0.096 Uiso 1 1 calc R
H17C H 0.2525 -0.0140 1.0212 0.096 Uiso 1 1 calc R
C18 C 0.2659(3) 0.04807(11) 0.8739(2) 0.0627(7) Uani 1 1 d .
H18A H 0.3164 0.0197 0.8675 0.094 Uiso 1 1 calc R
H18B H 0.3087 0.0749 0.8491 0.094 Uiso 1 1 calc R
H18C H 0.1688 0.0453 0.8242 0.094 Uiso 1 1 calc R
C19 C 0.4144(2) 0.05872(7) 1.0705(2) 0.0414(5) Uani 1 1 d .
H19A H 0.4690 0.0321 1.0569 0.050 Uiso 1 1 calc R
H19B H 0.4148 0.0568 1.1518 0.050 Uiso 1 1 calc R
C20 C 0.4851(2) 0.10337(7) 1.0554(2) 0.0385(5) Uani 1 1 d .
H20A H 0.5787 0.1044 1.1143 0.046 Uiso 1 1 calc R
H20B H 0.4972 0.1032 0.9780 0.046 Uiso 1 1 calc R
C21 C 0.4081(2) 0.15070(8) 1.18499(18) 0.0437(6) Uani 1 1 d .
H21A H 0.5036 0.1540 1.2375 0.066 Uiso 1 1 calc R
H21B H 0.3656 0.1231 1.2068 0.066 Uiso 1 1 calc R
H21C H 0.3543 0.1784 1.1906 0.066 Uiso 1 1 calc R
C22 C 0.4712(2) 0.18665(7) 1.03130(18) 0.0334(5) Uani 1 1 d .
H22A H 0.4767 0.1814 0.9526 0.040 Uiso 1 1 calc R
H22B H 0.5672 0.1904 1.0851 0.040 Uiso 1 1 calc R
C23 C 0.3911(2) 0.23142(7) 1.03070(18) 0.0349(5) Uani 1 1 d .
H23A H 0.4014 0.2401 1.1118 0.042 Uiso 1 1 calc R
H23B H 0.4325 0.2567 0.9973 0.042 Uiso 1 1 calc R
C24 C 0.2205(2) 0.22512(8) 0.84034(18) 0.0459(6) Uani 1 1 d .
H24A H 0.1206 0.2238 0.7982 0.069 Uiso 1 1 calc R
H24B H 0.2654 0.1970 0.8237 0.069 Uiso 1 1 calc R
H24C H 0.2604 0.2527 0.8156 0.069 Uiso 1 1 calc R
C25 C 0.1677(2) 0.26777(8) 0.9901(2) 0.0433(5) Uani 1 1 d .
H25A H 0.2047 0.2967 0.9689 0.065 Uiso 1 1 calc R
H25B H 0.1791 0.2682 1.0732 0.065 Uiso 1 1 calc R
H25C H 0.0688 0.2651 0.9453 0.065 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'
K K 0.2009 0.2494 '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
N1 K N2 100.87(5)
N1 K N3 109.77(5)
N2 K N3 62.60(5)
N1 K N4 113.12(5)
N2 K N4 121.45(5)
N3 K N4 61.61(4)
N1 K P 75.53(3)
N2 K P 107.09(4)
N3 K P 168.77(4)
N4 K P 126.31(3)
N1 K C8 67.93(4)
N2 K C8 138.49(5)
N3 K C8 158.64(5)
N4 K C8 98.98(5)
P K C8 32.28(3)
C24 K C8 94.43(5)
C8 P C1 104.42(8)
C8 P K 75.46(5)
C1 P K 124.55(6)
C16 N1 C15 108.93(17)
C16 N1 C14 109.57(15)
C15 N1 C14 110.31(15)
C16 N1 K 118.38(13)
C15 N1 K 103.73(12)
C14 N1 K 105.67(10)
C18 N2 C17 109.4(2)
C18 N2 C19 111.45(17)
C17 N2 C19 109.52(18)
C18 N2 K 97.77(14)
C17 N2 K 113.87(14)
C19 N2 K 114.26(12)
C21 N3 C22 110.48(16)
C21 N3 C20 110.11(16)
C22 N3 C20 110.48(15)
C21 N3 K 96.07(11)
C22 N3 K 114.64(11)
C20 N3 K 114.19(11)
C24 N4 C23 111.23(17)
C24 N4 C25 110.26(16)
C23 N4 C25 110.19(16)
C24 N4 K 91.19(12)
C23 N4 K 116.84(11)
C25 N4 K 115.62(13)
C2 Si1 C1 111.94(10)
C2 Si1 C3 109.37(11)
C1 Si1 C3 109.75(10)
C2 Si1 C4 107.32(12)
C1 Si1 C4 112.69(10)
C3 Si1 C4 105.51(11)
C7 Si2 C1 111.62(9)
C7 Si2 C5 109.20(10)
C1 Si2 C5 110.39(9)
C7 Si2 C6 107.22(12)
C1 Si2 C6 113.05(10)
C5 Si2 C6 105.08(10)
Si1 C1 Si2 121.39(10)
Si1 C1 P 108.67(9)
Si2 C1 P 107.07(9)
C9 C8 C13 115.09(17)
C9 C8 P 125.41(14)
C13 C8 P 119.50(14)
C9 C8 K 116.62(12)
C13 C8 K 82.44(10)
P C8 K 72.26(6)
C10 C9 C8 123.07(19)
C9 C10 C11 120.99(19)
C10 C11 C12 117.87(18)
C11 C12 C13 122.79(19)
C12 C13 C8 120.18(17)
C12 C13 C14 118.97(17)
C8 C13 C14 120.67(16)
N1 C14 C13 115.04(15)
N2 C19 C20 114.01(17)
N3 C20 C19 113.96(17)
N3 C22 C23 113.62(16)
N4 C23 C22 113.51(16)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
K N1 2.8008(16)
K N2 2.8565(17)
K N3 2.8590(15)
K N4 2.8725(17)
K P 3.2326(6)
K C8 3.2854(17)
P C8 1.8127(19)
P C1 1.9080(18)
N1 C16 1.456(3)
N1 C15 1.459(2)
N1 C14 1.477(2)
N2 C18 1.444(3)
N2 C17 1.462(3)
N2 C19 1.463(3)
N3 C21 1.457(3)
N3 C22 1.464(2)
N3 C20 1.468(2)
N4 C24 1.457(3)
N4 C23 1.465(2)
N4 C25 1.466(3)
Si1 C2 1.866(2)
Si1 C1 1.870(2)
Si1 C3 1.874(2)
Si1 C4 1.879(2)
Si2 C7 1.868(2)
Si2 C1 1.8705(19)
Si2 C5 1.874(2)
Si2 C6 1.884(2)
C8 C9 1.422(3)
C8 C13 1.436(2)
C9 C10 1.377(3)
C10 C11 1.382(3)
C11 C12 1.386(3)
C12 C13 1.391(3)
C13 C14 1.505(2)
C19 C20 1.510(3)
C22 C23 1.521(3)
