#------------------------------------------------------------------------------
#$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $
#$Revision: 120677 $
#$URL: svn://www.crystallography.net/cod/cif/1/10/09/1100901.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_1100901
_chemical_formula_moiety           'C48 H93 Ge K N3 P3 Si6'
_chemical_formula_sum     'C48 H93 Ge K N3 P3 Si6'
_chemical_formula_weight          1085.39
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'
 'Ge'  'Ge'   0.1547   1.8001
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting            cubic
_symmetry_space_group_name_H-M    'P a -3'
loop_
 _symmetry_equiv_pos_as_xyz
 'x, y, z'
 '-x+1/2, -y, z+1/2'
 '-x, y+1/2, -z+1/2'
 'x+1/2, -y+1/2, -z'
 'z, x, y'
 'z+1/2, -x+1/2, -y'
 '-z+1/2, -x, y+1/2'
 '-z, x+1/2, -y+1/2'
 'y, z, x'
 '-y, z+1/2, -x+1/2'
 'y+1/2, -z+1/2, -x'
 '-y+1/2, -z, x+1/2'
 '-x, -y, -z'
 'x-1/2, y, -z-1/2'
 'x, -y-1/2, z-1/2'
 '-x-1/2, y-1/2, z'
 '-z, -x, -y'
 '-z-1/2, x-1/2, y'
 'z-1/2, x, -y-1/2'
 'z, -x-1/2, y-1/2'
 '-y, -z, -x'
 'y, -z-1/2, x-1/2'
 '-y-1/2, z-1/2, x'
 'y-1/2, z, -x-1/2'
_cell_length_a                    23.4873(5)
_cell_length_b                    23.4873(5)
_cell_length_c                    23.4873(5)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      12956.8(5)
_cell_formula_units_Z             8
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     30903
_cell_measurement_theta_min       2.50
_cell_measurement_theta_max       26.37
_exptl_crystal_description        block
_exptl_crystal_colour             red
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.30
_exptl_crystal_size_min           0.20
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.113
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              4656
_exptl_absorpt_coefficient_mu     0.753
_exptl_absorpt_correction_type    multi-scan
_exptl_absorpt_correction_T_min   0.806
_exptl_absorpt_correction_T_max   0.864
_exptl_absorpt_process_details    SADABS
_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method        'thin-slice \w scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             202438
_diffrn_reflns_av_R_equivalents   0.0556
_diffrn_reflns_av_sigmaI/netI     0.0123
_diffrn_reflns_limit_h_min        -29
_diffrn_reflns_limit_h_max        29
_diffrn_reflns_limit_k_min        -29
_diffrn_reflns_limit_k_max        29
_diffrn_reflns_limit_l_min        -29
_diffrn_reflns_limit_l_max        29
_diffrn_reflns_theta_min          1.94
_diffrn_reflns_theta_max          26.37
_reflns_number_total              4426
_reflns_number_gt                 3729
_reflns_threshold_expression      I>2\s(I)
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+19.0115P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4426
_refine_ls_number_parameters      195
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0548
_refine_ls_R_factor_gt            0.0402
_refine_ls_wR_factor_ref          0.1358
_refine_ls_wR_factor_gt           0.1185
_refine_ls_goodness_of_fit_ref    1.167
_refine_ls_restrained_S_all       1.167
_refine_ls_shift/su_max           0.256
_refine_ls_shift/su_mean          0.003
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
 _atom_site_disorder_assembly
 _atom_site_disorder_group
Ge Ge 0.819965(11) 0.319965(11) 0.180035(11) 0.02177(15) Uani 1 3 d S . .
K K 0.91096(2) 0.41096(2) 0.08904(2) 0.0253(2) Uani 1 3 d S . .
Si1 Si 0.89370(4) 0.17590(3) 0.23722(4) 0.0323(2) Uani 1 1 d . . .
Si2 Si 1.01585(4) 0.22601(4) 0.20647(4) 0.0345(2) Uani 1 1 d . . .
P P 0.91576(3) 0.28923(3) 0.15138(3) 0.02098(17) Uani 1 1 d . . .
N N 0.98000(11) 0.33927(12) 0.01621(11) 0.0333(6) Uani 1 1 d . . .
C1 C 0.93618(12) 0.23989(11) 0.21140(12) 0.0254(6) Uani 1 1 d . . .
H1 H 0.9340 0.2659 0.2451 0.030 Uiso 1 1 calc R . .
C2 C 0.90495(19) 0.17005(19) 0.31620(15) 0.0530(10) Uani 1 1 d . . .
H2A H 0.8899 0.2041 0.3350 0.079 Uiso 1 1 calc R . .
H2B H 0.9458 0.1667 0.3242 0.079 Uiso 1 1 calc R . .
H2C H 0.8851 0.1363 0.3306 0.079 Uiso 1 1 calc R . .
C3 C 0.91822(17) 0.10833(14) 0.20289(17) 0.0468(9) Uani 1 1 d . . .
H3A H 0.8951 0.0765 0.2167 0.070 Uiso 1 1 calc R . .
H3B H 0.9583 0.1016 0.2125 0.070 Uiso 1 1 calc R . .
H3C H 0.9142 0.1115 0.1615 0.070 Uiso 1 1 calc R . .
C4 C 0.81431(15) 0.17780(15) 0.23068(18) 0.0473(9) Uani 1 1 d . . .
H4A H 0.7975 0.1502 0.2571 0.071 Uiso 1 1 calc R . .
H4B H 0.8033 0.1681 0.1916 0.071 Uiso 1 1 calc R . .
H4C H 0.8005 0.2161 0.2399 0.071 Uiso 1 1 calc R . .
C5 C 1.03731(16) 0.18207(16) 0.14345(18) 0.0514(9) Uani 1 1 d . . .
H5A H 1.0147 0.1933 0.1103 0.077 Uiso 1 1 calc R . .
H5B H 1.0307 0.1417 0.1517 0.077 Uiso 1 1 calc R . .
H5C H 1.0778 0.1882 0.1354 0.077 Uiso 1 1 calc R . .
C6 C 1.04355(16) 0.18671(17) 0.27067(17) 0.0508(9) Uani 1 1 d . . .
H6A H 1.0246 0.1497 0.2735 0.076 Uiso 1 1 calc R . .
H6B H 1.0358 0.2090 0.3051 0.076 Uiso 1 1 calc R . .
H6C H 1.0847 0.1810 0.2668 0.076 Uiso 1 1 calc R . .
C7 C 1.05448(16) 0.29574(16) 0.20480(18) 0.0492(9) Uani 1 1 d . . .
H7A H 1.0956 0.2888 0.2052 0.074 Uiso 1 1 calc R . .
H7B H 1.0439 0.3183 0.2382 0.074 Uiso 1 1 calc R . .
H7C H 1.0442 0.3165 0.1701 0.074 Uiso 1 1 calc R . .
C8 C 0.90534(12) 0.24114(11) 0.08962(12) 0.0255(6) Uani 1 1 d . . .
C9 C 0.86135(14) 0.20096(12) 0.08822(14) 0.0337(7) Uani 1 1 d . . .
H9 H 0.8352 0.1994 0.1190 0.040 Uiso 1 1 calc R . .
C10 C 0.85485(17) 0.16348(15) 0.04325(17) 0.0473(9) Uani 1 1 d . . .
H10 H 0.8244 0.1369 0.0434 0.057 Uiso 1 1 calc R . .
C11 C 0.89260(19) 0.16460(17) -0.00189(17) 0.0556(10) Uani 1 1 d . . .
H11 H 0.8887 0.1386 -0.0326 0.067 Uiso 1 1 calc R . .
C12 C 0.93587(17) 0.20399(15) -0.00147(15) 0.0453(8) Uani 1 1 d . . .
H12 H 0.9619 0.2047 -0.0324 0.054 Uiso 1 1 calc R . .
C13 C 0.94279(13) 0.24276(12) 0.04270(12) 0.0310(6) Uani 1 1 d . . .
C14 C 0.99300(13) 0.28268(13) 0.03989(13) 0.0332(6) Uani 1 1 d . . .
H14A H 1.0085 0.2876 0.0788 0.040 Uiso 1 1 calc R . .
H14B H 1.0231 0.2648 0.0164 0.040 Uiso 1 1 calc R . .
C15 C 1.03105(16) 0.37408(17) 0.02015(18) 0.0514(9) Uani 1 1 d . . .
H15A H 1.0612 0.3572 -0.0033 0.077 Uiso 1 1 calc R . .
H15B H 1.0436 0.3759 0.0599 0.077 Uiso 1 1 calc R . .
H15C H 1.0227 0.4126 0.0065 0.077 Uiso 1 1 calc R . .
C16 C 0.96272(16) 0.33483(17) -0.04341(14) 0.0465(8) Uani 1 1 d . . .
H16A H 0.9543 0.3729 -0.0583 0.070 Uiso 1 1 calc R . .
H16B H 0.9287 0.3109 -0.0463 0.070 Uiso 1 1 calc R . .
H16C H 0.9936 0.3177 -0.0656 0.070 Uiso 1 1 calc R . .
loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
Ge 0.02177(15) 0.02177(15) 0.02177(15) 0.00194(10) 0.00194(10) -0.00194(10)
K 0.0253(2) 0.0253(2) 0.0253(2) 0.0034(2) 0.0034(2) -0.0034(2)
Si1 0.0370(5) 0.0249(4) 0.0350(5) 0.0092(3) -0.0045(3) -0.0036(3)
Si2 0.0271(4) 0.0316(4) 0.0448(5) 0.0084(4) -0.0102(4) -0.0003(3)
P 0.0224(3) 0.0184(3) 0.0221(3) 0.0012(2) -0.0007(2) 0.0000(2)
N 0.0315(13) 0.0386(14) 0.0298(13) 0.0017(11) 0.0070(10) -0.0009(11)
C1 0.0285(14) 0.0216(13) 0.0261(13) 0.0030(10) -0.0054(11) -0.0006(10)
C2 0.062(2) 0.061(2) 0.0365(19) 0.0144(17) -0.0016(17) -0.0064(19)
C3 0.055(2) 0.0267(16) 0.058(2) 0.0034(15) -0.0095(17) -0.0032(15)
C4 0.0382(18) 0.0411(19) 0.063(2) 0.0228(17) 0.0005(16) -0.0114(14)
C5 0.0409(19) 0.048(2) 0.066(3) 0.0043(18) 0.0014(18) 0.0158(16)
C6 0.045(2) 0.049(2) 0.058(2) 0.0168(17) -0.0231(17) -0.0026(16)
C7 0.0392(19) 0.047(2) 0.061(2) 0.0112(17) -0.0156(17) -0.0121(16)
C8 0.0297(14) 0.0201(12) 0.0267(13) -0.0010(10) -0.0061(11) 0.0036(10)
C9 0.0382(16) 0.0241(14) 0.0388(16) 0.0015(12) -0.0054(13) -0.0023(12)
C10 0.053(2) 0.0314(16) 0.058(2) -0.0057(15) -0.0158(18) -0.0109(15)
C11 0.073(3) 0.046(2) 0.048(2) -0.0233(17) -0.0084(19) -0.0005(19)
C12 0.058(2) 0.0452(19) 0.0327(17) -0.0152(15) 0.0003(15) 0.0031(16)
C13 0.0346(15) 0.0302(15) 0.0282(14) -0.0031(12) -0.0028(12) 0.0042(12)
C14 0.0285(14) 0.0424(17) 0.0286(14) -0.0014(13) 0.0051(12) 0.0059(13)
C15 0.0419(19) 0.053(2) 0.059(2) 0.0047(18) 0.0096(17) -0.0116(17)
C16 0.050(2) 0.058(2) 0.0306(17) 0.0076(15) 0.0032(15) 0.0016(17)
_cod_database_code 1100901
_journal_paper_doi 10.1021/om0501125