#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/60/4116053.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_4116053
loop_
_publ_author_name
'Jianmin Li'
'Yanxiong Ke'
'Yugen Zhang'
'Gaofei He'
'Zheng Jiang'
'Masayoshi Nishiura'
'Tsuneo Imamoto'
_publ_section_title
;
 ((DABCO).ZnGe(HPO4)3: The First Zinco-Germanophosphate with a Unique
 Asymmetric Cage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6110
_journal_page_last               6111
_journal_paper_doi               10.1021/ja000107m
_journal_volume                  122
_journal_year                    2000
_chemical_formula_sum            'C6 H15 Ge N2 O12 P3 Zn'
_chemical_formula_weight         538.08
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                97.96(3)
_cell_angle_beta                 114.87(3)
_cell_angle_gamma                107.67(2)
_cell_formula_units_Z            2
_cell_length_a                   9.982(6)
_cell_length_b                   10.000(1)
_cell_length_c                   9.576(4)
_cell_measurement_temperature    288.2
_cell_volume                     786.2(7)
_computing_cell_refinement       PROCESS
_computing_data_collection       PROCESS
_computing_data_reduction        'teXsan Ver. 1.10'
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 0.010000
_diffrn_measured_fraction_theta_full 0.7939
_diffrn_measured_fraction_theta_max 0.7939
_diffrn_measurement_device_type  'Rigaku RAXIS-II Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2858
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_exptl_absorpt_coefficient_mu    3.809
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.273
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.350
_refine_diff_density_max         1.31
_refine_diff_density_min         -1.70
_refine_ls_extinction_coef       0.12(1)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 gaussian isotropic'
_refine_ls_goodness_of_fit_ref   3.192
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2799
_refine_ls_R_factor_gt           0.0685
_refine_ls_shift/su_max          0.0079
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w =3D 1/[σ²(Fo) + 0.00123|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                2799
_reflns_number_total             2858
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ja000107m.cif
_cod_data_source_block           ZnGePO4
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C6 H15 Ge N2 O12 P3 Zn '
_cod_database_code               4116053
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_calc_flag
Ge(1) Ge 0.03306(8) 0.11545(7) -0.13641(8) 0.0342(3) Uani 1.00 d
Zn(1) Zn 0.79116(8) 0.34102(7) 0.31218(8) 0.0288(3) Uani 1.00 d
P(1) P 0.4002(2) 0.2291(2) 0.1746(2) 0.0292(4) Uani 1.00 d
P(2) P 1.0284(2) 0.6595(2) 0.3362(2) 0.0301(4) Uani 1.00 d
P(3) P 0.9699(2) 0.1929(2) 0.1539(2) 0.0301(4) Uani 1.00 d
O(1) O 0.5573(5) 0.2874(5) 0.1695(5) 0.033(1) Uani 1.00 d
O(2) O 0.3955(6) 0.3338(5) 0.3021(6) 0.040(1) Uani 1.00 d
O(3) O 0.2638(5) 0.1943(5) 0.0052(5) 0.035(1) Uani 1.00 d
O(4) O 0.3841(6) 0.0786(6) 0.2199(6) 0.045(1) Uani 1.00 d
O(5) O 0.8875(6) 0.5486(5) 0.3392(7) 0.042(1) Uani 1.00 d
O(6) O 0.9972(6) 0.7954(5) 0.3046(5) 0.034(1) Uani 1.00 d
O(7) O 1.1864(6) 0.7022(6) 0.4937(6) 0.041(1) Uani 1.00 d
O(8) O 1.0473(6) 0.5915(5) 0.1887(6) 0.038(1) Uani 1.00 d
O(9) O 0.8407(6) 0.2212(5) 0.1787(6) 0.041(1) Uani 1.00 d
O(10) O 1.1175(5) 0.3481(5) 0.2204(6) 0.037(1) Uani 1.00 d
O(11) O 1.0364(6) 0.0933(5) 0.2445(6) 0.040(1) Uani 1.00 d
O(12) O 0.9061(6) 0.1294(5) -0.0283(5) 0.037(1) Uani 1.00 d
N(1) N 0.6016(7) 0.7727(6) 0.4437(7) 0.037(1) Uani 1.00 d
N(2) N 0.5200(7) 0.7456(6) 0.1520(7) 0.037(1) Uani 1.00 d
C(1) C 0.6054(8) 0.6511(7) 0.2051(8) 0.036(2) Uani 1.00 d
C(2) C 0.676(1) 0.6841(9) 0.3873(9) 0.045(2) Uani 1.00 d
C(3) C 0.6571(10) 0.9224(9) 0.4260(10) 0.051(2) Uani 1.00 d
C(4) C 0.6314(9) 0.9057(8) 0.2540(10) 0.043(2) Uani 1.00 d
C(5) C 0.3710(9) 0.7015(9) 0.1705(10) 0.046(2) Uani 1.00 d
C(6) C 0.4204(10) 0.695(1) 0.341(1) 0.054(2) Uani 1.00 d
H(1) H 1.0776 0.5027 0.1922 0.0560 Uiso 1.00 calc
H(2) H 1.2055 0.4406 0.2601 0.0442 Uiso 1.00 calc
H(3) H 0.3924 0.3995 0.3816 0.0483 Uiso 1.00 calc
H(4) H 0.5328 0.5503 0.1523 0.0429 Uiso 1.00 calc
H(5) H 0.6902 0.6705 0.1793 0.0429 Uiso 1.00 calc
H(6) H 0.6526 0.5936 0.4131 0.0529 Uiso 1.00 calc
H(7) H 0.7893 0.7376 0.4403 0.0529 Uiso 1.00 calc
H(8) H 0.7684 0.9763 0.5023 0.0617 Uiso 1.00 calc
H(9) H 0.5967 0.9730 0.4446 0.0617 Uiso 1.00 calc
H(10) H 0.5832 0.9688 0.2099 0.0522 Uiso 1.00 calc
H(11) H 0.7317 0.9291 0.2559 0.0522 Uiso 1.00 calc
H(12) H 0.2934 0.6085 0.0945 0.0551 Uiso 1.00 calc
H(13) H 0.3262 0.7737 0.1522 0.0551 Uiso 1.00 calc
H(14) H 0.3718 0.7426 0.3861 0.0653 Uiso 1.00 calc
H(15) H 0.3873 0.5952 0.3402 0.0653 Uiso 1.00 calc
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
H H 0.000 0.000
;International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.2)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Ge Ge 0.155 1.800
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
P P 0.102 0.094
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
Zn Zn 0.284 1.430
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O(3) Ge(1) O(6) 105.5(2) 1_555 2_665 yes
O(3) Ge(1) O(11) 107.2(2) 1_555 2_655 yes
O(3) Ge(1) O(12) 115.2(2) 1_555 1_455 yes
O(6) Ge(1) O(11) 104.4(2) 2_665 2_655 yes
O(6) Ge(1) O(12) 115.8(2) 2_665 1_455 yes
O(11) Ge(1) O(12) 108.0(2) 2_655 1_455 yes
O(1) Zn(1) O(5) 103.0(2) 1_555 1_555 yes
O(1) Zn(1) O(7) 106.7(2) 1_555 2_766 yes
O(1) Zn(1) O(9) 102.3(2) 1_555 1_555 yes
O(5) Zn(1) O(7) 114.3(2) 1_555 2_766 yes
O(5) Zn(1) O(9) 112.4(2) 1_555 1_555 yes
O(7) Zn(1) O(9) 116.2(2) 2_766 1_555 yes
O(1) P(1) O(2) 113.1(3) 1_555 1_555 yes
O(1) P(1) O(3) 107.1(3) 1_555 1_555 yes
O(1) P(1) O(4) 107.6(3) 1_555 1_555 yes
O(2) P(1) O(3) 112.8(3) 1_555 1_555 yes
O(2) P(1) O(4) 107.4(3) 1_555 1_555 yes
O(3) P(1) O(4) 108.6(3) 1_555 1_555 yes
O(5) P(2) O(6) 111.0(3) 1_555 1_555 yes
O(5) P(2) O(7) 111.0(3) 1_555 1_555 yes
O(5) P(2) O(8) 110.1(3) 1_555 1_555 yes
O(6) P(2) O(7) 111.1(3) 1_555 1_555 yes
O(6) P(2) O(8) 104.8(3) 1_555 1_555 yes
O(7) P(2) O(8) 108.6(3) 1_555 1_555 yes
O(9) P(3) O(10) 107.2(3) 1_555 1_555 yes
O(9) P(3) O(11) 115.1(3) 1_555 1_555 yes
O(9) P(3) O(12) 109.2(3) 1_555 1_555 yes
O(10) P(3) O(11) 106.6(3) 1_555 1_555 yes
O(10) P(3) O(12) 108.3(3) 1_555 1_555 yes
O(11) P(3) O(12) 110.2(3) 1_555 1_555 yes
Zn(1) O(1) P(1) 138.8(3) 1_555 1_555 yes
Ge(1) O(3) P(1) 146.6(3) 1_555 1_555 yes
Zn(1) O(5) P(2) 140.6(3) 1_555 1_555 yes
Ge(1) O(6) P(2) 136.0(3) 2_665 1_555 yes
Zn(1) O(7) P(2) 126.9(3) 2_766 1_555 yes
Zn(1) O(9) P(3) 146.8(3) 1_555 1_555 yes
Ge(1) O(11) P(3) 121.9(3) 2_655 1_555 yes
Ge(1) O(12) P(3) 127.3(3) 1_655 1_555 yes
C(2) N(1) C(3) 109.5(6) 1_555 1_555 yes
C(2) N(1) C(6) 108.6(6) 1_555 1_555 yes
C(3) N(1) C(6) 109.6(6) 1_555 1_555 yes
C(1) N(2) C(4) 109.3(5) 1_555 1_555 yes
C(1) N(2) C(5) 110.3(5) 1_555 1_555 yes
C(4) N(2) C(5) 109.5(5) 1_555 1_555 yes
N(2) C(1) C(2) 108.9(5) 1_555 1_555 yes
N(1) C(2) C(1) 109.1(6) 1_555 1_555 yes
N(1) C(3) C(4) 108.8(6) 1_555 1_555 yes
N(2) C(4) C(3) 107.8(6) 1_555 1_555 yes
N(2) C(5) C(6) 108.0(6) 1_555 1_555 yes
N(1) C(6) C(5) 109.3(6) 1_555 1_555 yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ge(1) O(3) 1.934(5) . yes
Ge(1) O(6) 1.906(4) 2_665 yes
Ge(1) O(11) 1.957(5) 2_655 yes
Ge(1) O(12) 1.967(5) 1_455 yes
Zn(1) O(1) 1.990(4) . yes
Zn(1) O(5) 1.931(4) . yes
Zn(1) O(7) 1.904(5) 2_766 yes
Zn(1) O(9) 1.945(5) . yes
P(1) O(1) 1.523(4) . yes
P(1) O(2) 1.521(5) . yes
P(1) O(3) 1.518(4) . yes
P(1) O(4) 1.604(5) . yes
P(2) O(5) 1.518(4) . yes
P(2) O(6) 1.526(4) . yes
P(2) O(7) 1.536(5) . yes
P(2) O(8) 1.591(5) . yes
P(3) O(9) 1.503(5) . yes
P(3) O(10) 1.592(5) . yes
P(3) O(11) 1.531(5) . yes
P(3) O(12) 1.538(5) . yes
N(1) C(2) 1.493(9) . yes
N(1) C(3) 1.49(1) . yes
N(1) C(6) 1.510(9) . yes
N(2) C(1) 1.462(8) . yes
N(2) C(4) 1.525(9) . yes
N(2) C(5) 1.510(9) . yes
C(1) C(2) 1.521(10) . yes
C(3) C(4) 1.53(1) . yes
C(5) C(6) 1.51(1) . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
P(1) N(2) 3.561(6) 2_665
P(3) O(2) 3.576(6) 1_655
O(1) N(2) 2.784(7) 2_665
O(1) C(1) 3.468(8) .
O(1) C(1) 3.493(8) 2_665
O(1) C(4) 3.595(9) 2_665
O(2) N(1) 2.782(8) 2_666
O(2) C(6) 3.23(1) 2_666
O(2) C(2) 3.353(9) 2_666
O(2) C(2) 3.479(10) .
O(2) C(6) 3.50(1) .
O(3) N(2) 3.079(8) 2_665
O(3) C(1) 3.162(8) 2_665
O(3) C(4) 3.222(9) 2_665
O(4) N(1) 3.282(8) 2_666
O(4) C(4) 3.355(10) 1_545
O(4) C(3) 3.560(10) 1_545
O(4) C(3) 3.58(1) 2_666
O(5) C(2) 2.982(9) .
O(5) C(1) 3.115(8) .
O(6) O(11) 3.052(7) 1_565
O(6) O(12) 3.280(6) 2_765
O(6) C(3) 3.334(9) 2_776
O(6) C(1) 3.368(8) .
O(6) C(2) 3.516(10) .
O(7) C(6) 3.246(10) 1_655
O(7) C(3) 3.429(10) 2_776
O(8) C(6) 3.121(10) 1_655
O(8) C(5) 3.170(9) 1_655
O(8) O(12) 3.371(7) 2_765
O(8) O(8) 3.399(10) 2_765
O(9) C(5) 3.466(10) 2_665
O(9) C(4) 3.568(9) 1_545
O(10) C(6) 3.480(10) 1_655
O(10) C(2) 3.563(9) 2_766
O(11) O(12) 3.174(7) 2_755
O(11) N(1) 3.263(7) 2_766
O(11) C(2) 3.326(9) 2_766
O(11) C(3) 3.413(9) 2_766
O(12) C(5) 3.560(9) 2_665
