#------------------------------------------------------------------------------
#$Date: 2018-09-01 22:33:33 +0300 (Sat, 01 Sep 2018) $
#$Revision: 210321 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/10/08/1100899.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_1100899
loop_
_publ_author_name
'Izod, Keith'
'McFarlane, William'
'Allen, Ben'
'Clegg, William'
'Harrington, Ross W.'
_publ_section_title
;
 An Intramolecularly Base-Stabilized Diphosphagermylene and Two Unusual
 Germanium(II) Ate Complexes: A Structural, NMR, and DFT Study
;
_journal_coden_ASTM              ORGND7
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2157
_journal_page_last               2167
_journal_paper_doi               10.1021/om0501125
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C32 H62 Ge N2 P2 Si4, 0.5 C7 H14'
_chemical_formula_sum            'C35.5 H69 Ge N2 P2 Si4'
_chemical_formula_weight         770.82
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                78.569(1)
_cell_angle_beta                 89.576(1)
_cell_angle_gamma                75.536(1)
_cell_formula_units_Z            2
_cell_length_a                   11.4596(5)
_cell_length_b                   12.0029(5)
_cell_length_c                   16.3524(7)
_cell_measurement_reflns_used    13588
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9
_cell_measurement_theta_min      2.16
_cell_volume                     2132.65(16)
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15612
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.737
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     413
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0268
_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)+(0.0417P)²+0.8715P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                8637
_reflns_number_total             9401
_reflns_threshold_expression     I>2σ(I)
_cod_database_code               1100899
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge Ge 0.339664(13) 0.041854(12) 0.179005(9) 0.01916(5) Uani 1 1 d . . .
P1 P 0.19237(3) 0.03927(3) 0.28420(2) 0.01874(8) Uani 1 1 d . . .
P2 P 0.47156(3) -0.13012(3) 0.26407(2) 0.01758(8) Uani 1 1 d . . .
Si1 Si -0.03479(4) 0.09811(4) 0.17835(3) 0.02998(10) Uani 1 1 d . . .
Si2 Si -0.02151(4) 0.25897(4) 0.30948(3) 0.02919(10) Uani 1 1 d . . .
Si3 Si 0.35557(4) -0.33940(4) 0.34097(3) 0.02924(10) Uani 1 1 d . . .
Si4 Si 0.40852(4) -0.30121(4) 0.14575(3) 0.02887(10) Uani 1 1 d . . .
N1 N 0.41870(12) 0.17393(11) 0.21553(8) 0.0244(3) Uani 1 1 d . . .
N2 N 0.81877(12) -0.38364(12) 0.37561(9) 0.0314(3) Uani 1 1 d . . .
C1 C 0.06320(13) 0.16638(13) 0.23583(9) 0.0224(3) Uani 1 1 d . . .
H1 H 0.0974 0.2195 0.1927 0.027 Uiso 1 1 calc R . .
C2 C -0.1314(2) 0.2119(2) 0.09383(16) 0.0634(7) Uani 1 1 d . . .
H2A H -0.1714 0.1733 0.0592 0.095 Uiso 1 1 calc R . .
H2B H -0.0809 0.2554 0.0591 0.095 Uiso 1 1 calc R . .
H2C H -0.1924 0.2663 0.1191 0.095 Uiso 1 1 calc R . .
C3 C -0.12808(17) 0.02272(19) 0.25303(14) 0.0437(5) Uani 1 1 d . . .
H3A H -0.1860 0.0811 0.2771 0.066 Uiso 1 1 calc R . .
H3B H -0.0755 -0.0335 0.2977 0.066 Uiso 1 1 calc R . .
H3C H -0.1717 -0.0191 0.2235 0.066 Uiso 1 1 calc R . .
C4 C 0.05627(17) -0.01435(19) 0.12280(12) 0.0403(4) Uani 1 1 d . . .
H4A H 0.1012 -0.0823 0.1639 0.060 Uiso 1 1 calc R . .
H4B H 0.1130 0.0198 0.0873 0.060 Uiso 1 1 calc R . .
H4C H 0.0023 -0.0394 0.0881 0.060 Uiso 1 1 calc R . .
C5 C -0.04985(18) 0.16944(19) 0.41147(12) 0.0441(5) Uani 1 1 d . . .
H5A H 0.0246 0.1423 0.4467 0.066 Uiso 1 1 calc R . .
H5B H -0.0761 0.1014 0.4015 0.066 Uiso 1 1 calc R . .
H5C H -0.1128 0.2177 0.4397 0.066 Uiso 1 1 calc R . .
C6 C 0.05901(17) 0.36965(16) 0.32954(13) 0.0400(4) Uani 1 1 d . . .
H6A H 0.0045 0.4284 0.3554 0.060 Uiso 1 1 calc R . .
H6B H 0.0849 0.4085 0.2766 0.060 Uiso 1 1 calc R . .
H6C H 0.1298 0.3299 0.3671 0.060 Uiso 1 1 calc R . .
C7 C -0.17277(17) 0.34883(19) 0.26168(15) 0.0492(5) Uani 1 1 d . . .
H7A H -0.2233 0.2964 0.2542 0.074 Uiso 1 1 calc R . .
H7B H -0.1620 0.3961 0.2073 0.074 Uiso 1 1 calc R . .
H7C H -0.2118 0.4008 0.2986 0.074 Uiso 1 1 calc R . .
C8 C 0.26477(13) 0.08112(12) 0.36949(9) 0.0206(3) Uani 1 1 d . . .
C9 C 0.25681(14) 0.01789(14) 0.45027(9) 0.0262(3) Uani 1 1 d . . .
H9 H 0.2091 -0.0374 0.4586 0.031 Uiso 1 1 calc R . .
C10 C 0.31723(16) 0.03437(16) 0.51840(10) 0.0328(4) Uani 1 1 d . . .
H10 H 0.3097 -0.0086 0.5727 0.039 Uiso 1 1 calc R . .
C11 C 0.38837(16) 0.11337(16) 0.50722(11) 0.0341(4) Uani 1 1 d . . .
H11 H 0.4314 0.1235 0.5535 0.041 Uiso 1 1 calc R . .
C12 C 0.39632(15) 0.17746(15) 0.42804(11) 0.0295(3) Uani 1 1 d . . .
H12 H 0.4446 0.2323 0.4205 0.035 Uiso 1 1 calc R . .
C13 C 0.33477(13) 0.16303(13) 0.35907(9) 0.0225(3) Uani 1 1 d . . .
C14 C 0.34186(14) 0.23746(12) 0.27455(10) 0.0238(3) Uani 1 1 d . . .
H14A H 0.2592 0.2702 0.2490 0.029 Uiso 1 1 calc R . .
H14B H 0.3739 0.3043 0.2820 0.029 Uiso 1 1 calc R . .
C15 C 0.4172(2) 0.26027(16) 0.13643(12) 0.0412(4) Uani 1 1 d . . .
H15A H 0.4517 0.3232 0.1472 0.062 Uiso 1 1 calc R . .
H15B H 0.3339 0.2938 0.1142 0.062 Uiso 1 1 calc R . .
H15C H 0.4652 0.2208 0.0957 0.062 Uiso 1 1 calc R . .
C16 C 0.54396(15) 0.12672(16) 0.25044(13) 0.0354(4) Uani 1 1 d . . .
H16A H 0.5954 0.0930 0.2087 0.053 Uiso 1 1 calc R . .
H16B H 0.5460 0.0656 0.3004 0.053 Uiso 1 1 calc R . .
H16C H 0.5736 0.1902 0.2654 0.053 Uiso 1 1 calc R . .
C17 C 0.38364(13) -0.23667(12) 0.24288(9) 0.0216(3) Uani 1 1 d . . .
H17 H 0.3012 -0.1828 0.2295 0.026 Uiso 1 1 calc R . .
C18 C 0.19067(19) -0.3334(2) 0.33874(15) 0.0562(6) Uani 1 1 d . . .
H18A H 0.1741 -0.3916 0.3855 0.084 Uiso 1 1 calc R . .
H18B H 0.1675 -0.3507 0.2860 0.084 Uiso 1 1 calc R . .
H18C H 0.1441 -0.2547 0.3436 0.084 Uiso 1 1 calc R . .
C19 C 0.4438(2) -0.49559(15) 0.34901(14) 0.0446(5) Uani 1 1 d . . .
H19A H 0.5299 -0.5010 0.3565 0.067 Uiso 1 1 calc R . .
H19B H 0.4297 -0.5220 0.2978 0.067 Uiso 1 1 calc R . .
H19C H 0.4179 -0.5455 0.3969 0.067 Uiso 1 1 calc R . .
C20 C 0.39359(19) -0.29639(17) 0.43906(11) 0.0392(4) Uani 1 1 d . . .
H20A H 0.3611 -0.3410 0.4866 0.059 Uiso 1 1 calc R . .
H20B H 0.3582 -0.2122 0.4351 0.059 Uiso 1 1 calc R . .
H20C H 0.4814 -0.3134 0.4470 0.059 Uiso 1 1 calc R . .
C21 C 0.55919(19) -0.40591(18) 0.14209(14) 0.0467(5) Uani 1 1 d . . .
H21A H 0.5599 -0.4423 0.0934 0.070 Uiso 1 1 calc R . .
H21B H 0.5743 -0.4671 0.1931 0.070 Uiso 1 1 calc R . .
H21C H 0.6223 -0.3632 0.1379 0.070 Uiso 1 1 calc R . .
C22 C 0.2886(2) -0.38089(18) 0.13589(14) 0.0485(5) Uani 1 1 d . . .
H22A H 0.2088 -0.3259 0.1328 0.073 Uiso 1 1 calc R . .
H22B H 0.2951 -0.4449 0.1846 0.073 Uiso 1 1 calc R . .
H22C H 0.2996 -0.4133 0.0851 0.073 Uiso 1 1 calc R . .
C23 C 0.38521(19) -0.18378(17) 0.04936(11) 0.0389(4) Uani 1 1 d . . .
H23A H 0.4531 -0.1471 0.0447 0.058 Uiso 1 1 calc R . .
H23B H 0.3101 -0.1242 0.0524 0.058 Uiso 1 1 calc R . .
H23C H 0.3802 -0.2183 0.0004 0.058 Uiso 1 1 calc R . .
C24 C 0.61238(13) -0.16292(12) 0.20656(9) 0.0196(3) Uani 1 1 d . . .
C25 C 0.62652(14) -0.09797(13) 0.12771(9) 0.0247(3) Uani 1 1 d . . .
H25 H 0.5606 -0.0365 0.1012 0.030 Uiso 1 1 calc R . .
C26 C 0.73447(16) -0.12081(15) 0.08702(10) 0.0304(3) Uani 1 1 d . . .
H26 H 0.7417 -0.0755 0.0335 0.036 Uiso 1 1 calc R . .
C27 C 0.83109(16) -0.21001(15) 0.12525(11) 0.0321(4) Uani 1 1 d . . .
H27 H 0.9048 -0.2267 0.0977 0.038 Uiso 1 1 calc R . .
C28 C 0.82011(15) -0.27496(14) 0.20372(10) 0.0286(3) Uani 1 1 d . . .
H28 H 0.8868 -0.3361 0.2295 0.034 Uiso 1 1 calc R . .
C29 C 0.71268(13) -0.25206(12) 0.24548(9) 0.0221(3) Uani 1 1 d . . .
C30 C 0.70313(14) -0.32623(14) 0.33028(10) 0.0270(3) Uani 1 1 d . . .
H30A H 0.6519 -0.2757 0.3646 0.032 Uiso 1 1 calc R . .
H30B H 0.6621 -0.3873 0.3230 0.032 Uiso 1 1 calc R . .
C31 C 0.87381(17) -0.29882(19) 0.40210(13) 0.0434(4) Uani 1 1 d . . .
H31A H 0.8222 -0.2600 0.4416 0.065 Uiso 1 1 calc R . .
H31B H 0.8830 -0.2399 0.3533 0.065 Uiso 1 1 calc R . .
H31C H 0.9532 -0.3395 0.4292 0.065 Uiso 1 1 calc R . .
C32 C 0.80028(18) -0.46803(18) 0.44877(12) 0.0469(5) Uani 1 1 d . . .
H32A H 0.8777 -0.5068 0.4792 0.070 Uiso 1 1 calc R . .
H32B H 0.7661 -0.5270 0.4310 0.070 Uiso 1 1 calc R . .
H32C H 0.7446 -0.4270 0.4853 0.070 Uiso 1 1 calc R . .
C33 C 0.1023(3) 0.4176(3) 0.0787(2) 0.0882(10) Uani 1 1 d . . .
H33A H 0.1755 0.4264 0.1058 0.106 Uiso 1 1 calc R . .
H33B H 0.0845 0.3414 0.1025 0.106 Uiso 1 1 calc R . .
C34 C 0.0014(3) 0.5166(3) 0.0706(3) 0.1000(12) Uani 1 1 d . . .
H34A H 0.0360 0.5852 0.0665 0.120 Uiso 1 1 calc R . .
H34B H -0.0368 0.5080 0.1252 0.120 Uiso 1 1 calc R . .
C35 C -0.0978(5) 0.5537(4) 0.0085(2) 0.1180(16) Uani 1 1 d . . .
H35A H -0.1416 0.4914 0.0215 0.142 Uiso 1 1 calc R . .
H35B H -0.1512 0.6237 0.0248 0.142 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'
P P 0.1023 0.0942 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
