#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/42/4314228.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_4314228
loop_
_publ_author_name
'Jacques Plévert'
'Rebeca Sanchez-Smith'
'Travis M. Gentz'
'Hailian Li'
'Thomas L. Groy'
'Omar M. Yaghi'
'Michael O'Keeffe'
_publ_contact_author_address
;
Jacques Plevert
Department of Chemistry & Biochemistry
Physical Sciences D-121
Arizona State University
Tempe, AZ 85287-1604  
USA
;
_publ_contact_author_email       JPlevert@asu.edu
_publ_contact_author_name        'Jacques Plevert'
_publ_section_title
;
 Synthesis and Characterization of Zirconogermanates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5954
_journal_page_last               5959
_journal_paper_doi               10.1021/ic034298g
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C10 H29 F Ge3 N4 O10 Zr'
_chemical_formula_weight         693.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'by teXsan'
_cell_angle_alpha                90
_cell_angle_beta                 97.936(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7957(8)
_cell_length_b                   12.700(1)
_cell_length_c                   24.293(3)
_cell_measurement_reflns_used    1873
_cell_measurement_temperature    159.2
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.0
_cell_volume                     2076.5(4)
_computing_cell_refinement       'Bruker SAINT v5.04'
_computing_data_collection       'Bruker SMART v5.0'
_computing_data_reduction        'Bruker SAINT v5.04'
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_measured_fraction_theta_full 0.9713
_diffrn_measured_fraction_theta_max 0.9713
_diffrn_measurement_device_type  'SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.037
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            3595
_diffrn_reflns_theta_full        24.72
_diffrn_reflns_theta_max         24.72
_exptl_absorpt_coefficient_mu    9.374
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.600
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.67
_refine_diff_density_min         -0.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.818
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     257
_refine_ls_number_reflns         2112
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(Fo) + 0.00022|Fo|²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0292
_reflns_number_gt                2112
_reflns_number_total             3419
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ic034298gsi20030318_100311_1.cif
_cod_data_source_block           ASU-23
_cod_original_cell_volume        2076.4(4)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C10 H29 F Ge3 N4 O10 Zr '
_cod_database_code               4314228
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
1/2-x,1/2+y,1/2-z
-x,-y,-z
1/2+x,1/2-y,1/2+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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.72073(10) 0.67074(5) 0.77902(3) 0.0076(2) Uani 1.00 d . . .
Ge1 Ge 0.1993(1) 0.71972(6) 0.74233(3) 0.0085(2) Uani 1.00 d . . .
Ge2 Ge 0.4386(1) 0.61822(6) 0.65686(3) 0.0097(2) Uani 1.00 d . . .
Ge3 Ge 0.5533(1) 0.41982(6) 0.73374(3) 0.0095(2) Uani 1.00 d . . .
F1 F 0.7767(5) 0.6589(3) 0.8629(2) 0.012(1) Uani 1.00 d . . .
O1 O 0.4214(6) 0.7018(3) 0.7859(2) 0.009(1) Uani 1.00 d . . .
O2 O 0.2214(6) 0.6797(4) 0.6738(2) 0.013(1) Uani 1.00 d . . .
O3 O 0.0121(6) 0.6466(3) 0.7651(2) 0.010(1) Uani 1.00 d . . .
O4 O 0.1364(6) 0.8545(3) 0.7356(2) 0.012(1) Uani 1.00 d . . .
O5 O 0.6494(6) 0.6712(4) 0.6941(2) 0.012(1) Uani 1.00 d . . .
O6 O 0.4173(6) 0.4835(3) 0.6754(2) 0.011(1) Uani 1.00 d . . .
O7 O 0.4277(6) 0.6191(4) 0.5851(2) 0.013(1) Uani 1.00 d . . .
O8 O 0.6622(6) 0.5109(3) 0.7804(2) 0.010(1) Uani 1.00 d . . .
O9 O 0.7194(6) 0.3311(3) 0.7128(2) 0.008(1) Uiso 1.00 d . . .
O10 O 0.5612(7) 0.6049(4) 0.9440(2) 0.021(2) Uani 1.00 d . . .
N1 N 0.6349(8) 0.7946(4) 0.5537(2) 0.011(2) Uani 1.00 d . . .
N2 N 0.8279(8) 0.7170(4) 0.4620(2) 0.011(2) Uani 1.00 d . . .
N3 N 0.1646(8) 1.0129(4) 0.6466(2) 0.013(2) Uani 1.00 d . . .
N4 N 1.0070(8) 0.5345(4) 0.3199(3) 0.011(2) Uani 1.00 d . . .
C1 C 0.845(1) 0.7670(5) 0.5605(3) 0.014(2) Uani 1.00 d . . .
C2 C 0.885(1) 0.6813(6) 0.5197(3) 0.017(2) Uani 1.00 d . . .
C3 C 0.617(1) 0.7444(6) 0.4559(3) 0.016(2) Uani 1.00 d . . .
C4 C 0.575(1) 0.8287(6) 0.4959(3) 0.017(2) Uani 1.00 d . . .
C5 C 0.6023(10) 0.8779(6) 0.5937(3) 0.012(2) Uani 1.00 d . . .
C6 C 0.383(1) 0.9021(5) 0.5963(3) 0.016(2) Uani 1.00 d . . .
C7 C 0.372(1) 0.9875(6) 0.6395(3) 0.014(2) Uani 1.00 d . . .
C8 C 0.853(1) 0.6336(6) 0.4218(3) 0.016(2) Uani 1.00 d . . .
C9 C 1.0704(10) 0.6090(5) 0.4157(3) 0.014(2) Uani 1.00 d . . .
C10 C 1.0887(10) 0.5148(6) 0.3788(3) 0.015(2) Uani 1.00 d . . .
H1 H 0.4921 0.6759 0.9514 0.0179 Uiso 1.00 calc . . .
H2 H 0.6291 0.6210 0.9157 0.0179 Uiso 1.00 calc . . .
H3 H 0.9206 0.8277 0.5542 0.0169 Uiso 1.00 calc . . .
H4 H 0.8844 0.7424 0.5974 0.0169 Uiso 1.00 calc . . .
H5 H 0.8099 0.6204 0.5261 0.0200 Uiso 1.00 calc . . .
H6 H 1.0224 0.6644 0.5252 0.0200 Uiso 1.00 calc . . .
H7 H 0.5768 0.7688 0.4191 0.0187 Uiso 1.00 calc . . .
H8 H 0.5427 0.6833 0.4623 0.0187 Uiso 1.00 calc . . .
H9 H 0.4362 0.8435 0.4906 0.0204 Uiso 1.00 calc . . .
H10 H 0.6460 0.8905 0.4891 0.0204 Uiso 1.00 calc . . .
H11 H 0.6619 0.8563 0.6296 0.0140 Uiso 1.00 calc . . .
H12 H 0.6647 0.9405 0.5835 0.0140 Uiso 1.00 calc . . .
H13 H 0.3213 0.9259 0.5610 0.0195 Uiso 1.00 calc . . .
H14 H 0.3176 0.8404 0.6065 0.0195 Uiso 1.00 calc . . .
H15 H 0.4339 1.0493 0.6282 0.0174 Uiso 1.00 calc . . .
H16 H 0.4402 0.9641 0.6741 0.0174 Uiso 1.00 calc . . .
H17 H 0.1088 0.9558 0.6645 0.0156 Uiso 1.00 calc . . .
H18 H 0.1626 1.0745 0.6687 0.0156 Uiso 1.00 calc . . .
H19 H 0.0890 1.0246 0.6113 0.0156 Uiso 1.00 calc . . .
H20 H 1.0777 0.5907 0.3059 0.0133 Uiso 1.00 calc . . .
H21 H 1.0206 0.4727 0.2987 0.0133 Uiso 1.00 calc . . .
H22 H 0.8705 0.5526 0.3175 0.0133 Uiso 1.00 calc . . .
H23 H 0.7938 0.5712 0.4334 0.0193 Uiso 1.00 calc . . .
H24 H 0.7868 0.6547 0.3866 0.0193 Uiso 1.00 calc . . .
H25 H 1.1266 0.6685 0.4000 0.0171 Uiso 1.00 calc . . .
H26 H 1.1414 0.5951 0.4514 0.0171 Uiso 1.00 calc . . .
H27 H 1.0188 0.4575 0.3921 0.0174 Uiso 1.00 calc . . .
H28 H 1.2253 0.4970 0.3807 0.0174 Uiso 1.00 calc . . .
H29 H 0.4648 0.6764 0.5721 0.0179 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
Zr Zr -2.967 0.560
;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)
;
O O 0.011 0.006
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
F F 0.017 0.010
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
N N 0.006 0.003
;International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1)
;
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)
;
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
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
F1 ZR1 O1 89.0(2) . . . ?
F1 ZR1 O3 95.9(2) . . . ?
F1 ZR1 O3 95.9(2) . . 1_655 ?
F1 ZR1 O5 175.1(2) . . . ?
F1 ZR1 O8 85.5(2) . . . ?
F1 ZR1 O9 88.2(2) . . . ?
F1 ZR1 O9 88.2(2) . . 2_656 ?
O1 ZR1 O3 174.7(2) . . . ?
O1 ZR1 O3 174.7(2) . . 1_655 ?
O1 ZR1 O5 89.0(2) . . . ?
O1 ZR1 O8 89.6(2) . . . ?
O1 ZR1 O9 89.3(2) . . . ?
O1 ZR1 O9 89.3(2) . . 2_656 ?
O3 ZR1 O5 86.3(2) . . . ?
O3 ZR1 O5 86.3(2) 1_655 . . ?
O3 ZR1 O8 92.7(2) . . . ?
O3 ZR1 O8 92.7(2) 1_655 . . ?
O3 ZR1 O9 89.0(2) 1_655 . 2_656 ?
O5 ZR1 O8 90.0(2) . . . ?
O5 ZR1 O9 96.3(2) . . . ?
O5 ZR1 O9 96.3(2) . . 2_656 ?
O8 ZR1 O9 173.6(2) . . . ?
O8 ZR1 O9 173.6(2) . . 2_656 ?
O1 GE1 O2 110.9(2) . . . ?
O1 GE1 O3 110.6(2) . . . ?
O1 GE1 O4 111.3(2) . . . ?
O2 GE1 O3 108.0(2) . . . ?
O2 GE1 O4 104.1(2) . . . ?
O3 GE1 O4 111.8(2) . . . ?
O2 GE2 O5 111.4(2) . . . ?
O2 GE2 O6 105.4(2) . . . ?
O2 GE2 O7 108.1(2) . . . ?
O5 GE2 O6 109.5(2) . . . ?
O5 GE2 O7 116.2(2) . . . ?
O6 GE2 O7 105.5(2) . . . ?
O4 GE3 O6 102.6(2) . . . ?
O4 GE3 O6 102.6(2) 2_546 . . ?
O4 GE3 O8 108.0(2) . . . ?
O4 GE3 O8 108.0(2) 2_546 . . ?
O4 GE3 O9 111.2(2) . . . ?
O4 GE3 O9 111.2(2) 2_546 . . ?
O6 GE3 O8 110.5(2) . . . ?
O6 GE3 O9 110.7(2) . . . ?
O8 GE3 O9 113.3(2) . . . ?
ZR1 O1 GE1 138.3(3) . . . ?
GE1 O2 GE2 122.0(3) . . . ?
ZR1 O3 GE1 137.2(2) . . . ?
ZR1 O3 GE1 137.2(2) 1_455 . . ?
GE1 O4 GE3 126.3(3) . . . ?
GE1 O4 GE3 126.3(3) . . 2_556 ?
ZR1 O5 GE2 126.2(2) . . . ?
GE2 O6 GE3 126.0(3) . . . ?
ZR1 O8 GE3 135.8(3) . . . ?
ZR1 O9 GE3 137.7(2) . . . ?
ZR1 O9 GE3 137.7(2) 2_646 . . ?
C1 N1 C4 108.6(5) . . . ?
C1 N1 C5 109.4(5) . . . ?
C4 N1 C5 111.7(5) . . . ?
C2 N2 C3 107.2(5) . . . ?
C2 N2 C8 111.8(6) . . . ?
C3 N2 C8 107.9(5) . . . ?
N1 C1 C2 110.9(6) . . . ?
N2 C2 C1 110.7(6) . . . ?
N2 C3 C4 112.1(6) . . . ?
N1 C4 C3 110.8(6) . . . ?
N1 C5 C6 114.0(6) . . . ?
C5 C6 C7 108.2(6) . . . ?
N3 C7 C6 112.1(6) . . . ?
N2 C8 C9 114.5(6) . . . ?
C8 C9 C10 112.2(6) . . . ?
N4 C10 C9 112.8(6) . . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
ZR1 F1 2.027(4) . . yes
ZR1 O1 2.101(4) . . yes
ZR1 O3 2.077(4) . 1_655 yes
ZR1 O5 2.053(5) . . yes
ZR1 O8 2.070(4) . . yes
ZR1 O9 2.081(4) . 2_656 yes
GE1 O1 1.735(4) . . yes
GE1 O2 1.766(5) . . yes
GE1 O3 1.726(4) . . yes
GE1 O4 1.767(4) . . yes
GE2 O2 1.768(4) . . yes
GE2 O5 1.722(4) . . yes
GE2 O6 1.780(4) . . yes
GE2 O7 1.735(5) . . yes
GE3 O4 1.780(4) . 2_546 yes
GE3 O6 1.776(4) . . yes
GE3 O8 1.715(4) . . yes
GE3 O9 1.721(4) . . yes
N1 C1 1.460(8) . . yes
N1 C4 1.472(9) . . yes
N1 C5 1.474(8) . . yes
N2 C2 1.473(9) . . yes
N2 C3 1.464(8) . . yes
N2 C8 1.466(9) . . yes
N3 C7 1.478(8) . . yes
N4 C10 1.482(9) . . yes
C1 C2 1.521(10) . . yes
C3 C4 1.501(10) . . yes
C5 C6 1.531(9) . . yes
C6 C7 1.519(10) . . yes
C8 C9 1.536(9) . . yes
C9 C10 1.510(10) . . yes
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
_geom_contact_publ_flag
GE1 GE3 3.165(1) . 2_556 ?
GE1 O9 3.485(4) . 2_556 ?
GE3 N4 3.470(5) . 3_766 ?
F1 O10 2.701(6) . . ?
F1 C7 3.238(8) . 2_646 ?
F1 C3 3.241(8) . 4_565 ?
F1 N3 3.506(7) . 2_546 ?
F1 C4 3.572(8) . 4_565 ?
F1 C9 3.576(8) . 4_465 ?
O1 N3 3.008(7) . 2_546 ?
O1 N4 3.479(7) . 4_465 ?
O2 N4 3.146(7) . 3_666 ?
O2 C10 3.381(9) . 3_666 ?
O3 O5 2.823(6) . 1_455 ?
O3 O9 2.914(6) . 2_556 ?
O3 O8 3.001(6) . 1_455 ?
O3 N4 3.081(7) . 3_666 ?
O3 C7 3.094(9) . 2_546 ?
O3 N3 3.319(7) . 2_546 ?
O4 O6 2.776(6) . 2_556 ?
O4 O8 2.827(6) . 2_556 ?
O4 O9 2.888(6) . 2_556 ?
O4 N3 2.978(7) . . ?
O4 N4 3.332(7) . 4_465 ?
O4 C7 3.448(8) . . ?
O5 N4 3.552(7) . 3_766 ?
O5 C5 3.567(8) . . ?
O5 C10 3.572(8) . 3_766 ?
O6 N4 2.910(7) . 3_666 ?
O6 C8 3.159(8) . 3_666 ?
O6 C10 3.508(8) . 3_666 ?
O7 N1 2.797(7) . . ?
O7 C5 3.490(8) . . ?
O7 C1 3.522(8) . . ?
O8 N3 3.026(7) . 2_546 ?
O8 C7 3.493(8) . 2_646 ?
O8 N4 3.583(7) . 3_766 ?
O9 N4 2.722(7) . 3_766 ?
O9 C10 3.359(9) . 3_766 ?
O10 N3 2.763(8) . 2_546 ?
O10 N2 2.831(7) . 4_465 ?
O10 C2 3.578(9) . 4_465 ?
C2 C10 3.49(1) . 3_766 ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 N2 60.3(7) . . . . ?
N1 C4 C3 N2 -59.4(8) . . . . ?
N1 C5 C6 C7 179.1(6) . . . . ?
N2 C8 C9 C10 173.6(6) . . . . ?
N3 C7 C6 C5 -177.5(5) . . . . ?
N4 C10 C9 C8 67.7(8) . . . . ?
C1 N1 C4 C3 56.9(7) . . . . ?
C1 N1 C5 C6 -171.6(6) . . . . ?
C1 C2 N2 C3 -58.5(7) . . . . ?
C1 C2 N2 C8 -176.5(5) . . . . ?
C2 N2 C3 C4 58.7(7) . . . . ?
C2 N2 C8 C9 -72.5(7) . . . . ?
C2 C1 N1 C4 -57.7(7) . . . . ?
C2 C1 N1 C5 -179.8(6) . . . . ?
C3 N2 C8 C9 169.8(6) . . . . ?
C3 C4 N1 C5 177.6(5) . . . . ?
C4 N1 C5 C6 68.2(7) . . . . ?
C4 C3 N2 C8 179.3(6) . . . . ?
