#------------------------------------------------------------------------------
#$Date: 2019-11-17 11:48:03 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229691 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/80/7048020.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_7048020
loop_
_publ_author_name
'Jo, Donghui'
'Choi, Wanuk'
'Shin, Jiho'
'Hong, Suk Bong'
_publ_section_title
;
 An open-framework silicogermanate regularly constructed from natrolite
 zeolite chains and Ge₉O₁₈(OH)₄ clusters.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17122
_journal_page_last               17126
_journal_paper_doi               10.1039/c8dt04175j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'Si2.63 Ge5.88 O21 H2, C8 H24 N2'
_chemical_formula_sum            'C8 H26 Ge5.88 N2 O21 Si2.63'
_chemical_formula_weight         1014.60
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2018-09-21 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.895(3)
_cell_length_b                   20.421(4)
_cell_length_c                   20.281(4)
_cell_measurement_reflns_used    24276
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.129
_cell_measurement_theta_min      1.629
_cell_volume                     5340.6(19)
_computing_cell_refinement       'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_data_collection       'PAL BL2D-SMDC Program'
_computing_data_reduction        'HKL3000sm (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    Mercury
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'MX225-HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.620
_diffrn_reflns_av_R_equivalents  0.1410
_diffrn_reflns_av_unetI/netI     0.1904
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4224
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        21.839
_diffrn_reflns_theta_max         21.129
_diffrn_reflns_theta_min         1.629
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    4.548
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.524
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3958
_exptl_crystal_size_max          0.010
_exptl_crystal_size_mid          0.000
_exptl_crystal_size_min          0.000
_refine_diff_density_max         1.710
_refine_diff_density_min         -3.314
_refine_diff_density_rms         0.360
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2272
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1983
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1792P)²+164.4099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3090
_refine_ls_wR_factor_ref         0.3558
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1058
_reflns_number_total             2272
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt04175j2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments          'Adding full bibliography for 7048020.cif.'
_cod_database_code               7048020
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.956
_shelx_estimated_absorpt_t_max   1.000
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.285(3) 0.3075(14) 0.1732(18) 0.103(16) Uani 1.0000(10) 1 d D U P . .
H1A H -0.3431 0.2934 0.1455 0.154 Uiso 1.0000(10) 1 calc R U P . .
H1B H -0.3070 0.3443 0.2009 0.154 Uiso 1.0000(10) 1 calc R U P . .
H1C H -0.2271 0.3213 0.1452 0.154 Uiso 1.0000(10) 1 calc R U P . .
C2 C -0.158(2) 0.2723(18) 0.2613(17) 0.14(2) Uani 1.0000(10) 1 d D U P . .
H2A H -0.1008 0.2863 0.2332 0.213 Uiso 1.0000(10) 1 calc R U P . .
H2B H -0.1806 0.3089 0.2892 0.213 Uiso 1.0000(10) 1 calc R U P . .
H2C H -0.1360 0.2358 0.2892 0.213 Uiso 1.0000(10) 1 calc R U P . .
C3 C -0.355(4) 0.518(3) 0.0000 0.12(2) Uani 1.0000(10) 2 d DS TU P . .
H3A H -0.4198 0.5018 0.0200 0.179 Uiso 0.500(1) 1 calc DR U P . .
H3B H -0.3690 0.5317 -0.0454 0.179 Uiso 0.500(1) 1 calc R U P . .
H3C H -0.3292 0.5551 0.0255 0.179 Uiso 0.500(1) 1 calc R U P . .
C4 C -0.291(3) 0.4228(18) -0.0601(13) 0.109(17) Uani 1.0000(10) 1 d D U P . .
H4A H -0.3608 0.4040 -0.0599 0.163 Uiso 1.0000(10) 1 calc R U P . .
H4B H -0.2819 0.4498 -0.0997 0.163 Uiso 1.0000(10) 1 calc R U P . .
H4C H -0.2395 0.3874 -0.0603 0.163 Uiso 1.0000(10) 1 calc R U P . .
C5 C -0.170(4) 0.493(2) 0.0000 0.081(15) Uani 1.0000(10) 2 d DS TU P . .
H5A H -0.1607 0.5200 0.0395 0.121 Uiso 0.500(1) 1 calc R U P . .
H5B H -0.1184 0.4577 0.0000 0.121 Uiso 1.0000(10) 2 calc R U P . .
H5C H -0.1608 0.5201 -0.0394 0.121 Uiso 0.500(1) 1 calc R U P . .
N1 N -0.2500 0.2500 0.2176(15) 0.055(10) Uani 1.0000(10) 2 d DS TU P . .
N2 N -0.276(2) 0.4642(15) 0.0000 0.071(12) Uani 1.0000(10) 2 d DS TU P . .
O1 O 0.1323(14) 0.3731(8) 0.1069(8) 0.022(4) Uani 1 1 d . U . . .
H1 H 0.1876 0.3518 0.1021 0.033 Uiso 1 1 calc R U . . .
O2 O -0.0674(14) 0.3657(8) 0.1262(9) 0.026(4) Uani 1 1 d . U . . .
O3 O -0.039(2) 0.3543(12) 0.0000 0.024(5) Uani 1 2 d S TU P . .
O4 O 0.0045(14) 0.2508(8) 0.1044(8) 0.018(3) Uani 1 1 d . U . . .
O5 O 0.1192(19) 0.2900(11) 0.0000 0.015(4) Uani 1 2 d S TU P . .
O6 O 0.2016(13) 0.1924(7) 0.0668(8) 0.015(3) Uani 1 1 d . U . . .
O7 O 0.317(3) 0.0463(17) 0.2987(16) 0.095(7) Uani 1 1 d . U . . .
O8 O 0.5000 0.093(2) 0.2500 0.089(8) Uani 1 2 d S TU P . .
O9 O 0.5000 0.0000 0.342(2) 0.086(8) Uani 1 2 d S TU P . .
O10 O 0.172(2) 0.0505(14) 0.2024(15) 0.074(6) Uani 1 1 d . U . . .
O11 O 0.0000 0.0916(13) 0.2500 0.050(7) Uani 1 2 d S TU P . .
O12 O 0.0000 0.0000 0.1531(14) 0.050(7) Uani 1 2 d S TU P . .
O13 O 0.0415(17) 0.1187(8) 0.1283(9) 0.037(4) Uani 1 1 d . U . . .
O14 O 0.014(2) 0.1561(11) 0.0000 0.019(4) Uani 1 2 d S TU P . .
T1 Si 0.0563(6) 0.0668(3) 0.1829(3) 0.0189(16) Uani 1 1 d . U . . .
T2SI Si 0.2484 0.0000 0.2500 0.078(3) Uani 0.5406(10) 2 d S TU P A 1
T3SI Si 0.4415 0.0676 0.3196 0.0643(19) Uani 0.5408(10) 1 d . U P A 1
T2GE Ge 0.2484 0.0000 0.2500 0.078(3) Uani 0.4594(10) 2 d S TU P A 2
T3GE Ge 0.4415 0.0676 0.3196 0.0643(19) Uani 0.4592(10) 1 d . U P A 2
Ge1 Ge 0.0692(2) 0.18328(13) 0.07370(14) 0.0212(8) Uani 1 1 d . U . . .
Ge2 Ge 0.2500 0.2500 0.0000 0.0086(12) Uani 1 4 d S TU P . .
Ge3 Ge 0.0293(2) 0.32951(13) 0.07164(13) 0.0179(8) Uani 1 1 d . U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 '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 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0640 0.0530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.2720 1.4270 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C2 N1 C2 110.0(11) . 6_455
C2 N1 C1 109.5(5) . 6_455
C2 N1 C1 109.4(5) 6_455 6_455
C2 N1 C1 109.4(5) . .
C2 N1 C1 109.5(5) 6_455 .
C1 N1 C1 108.9(11) 6_455 .
C5 N2 C4 109.8(8) . .
C5 N2 C4 109.8(8) . 10
C4 N2 C4 109.2(12) . 10
C5 N2 C3 109.8(12) . .
C4 N2 C3 109.1(8) . .
C4 N2 C3 109.1(8) 10 .
T3GE O2 Ge3 130.5(11) 8_455 .
T3SI O2 Ge3 130.5(11) 8_455 .
Ge3 O3 Ge3 110.2(13) 10 .
Ge1 O4 Ge3 120.2(10) . .
Ge2 O5 Ge3 133.5(5) . 10
Ge2 O5 Ge3 133.5(5) . .
Ge3 O5 Ge3 91.6(10) 10 .
Ge1 O6 Ge2 116.8(8) . .
T2GE O7 T3GE 144(2) . .
T2SI O7 T3SI 144(2) . .
T3SI O8 T3SI 144(3) 3_655 .
T3GE O8 T3GE 144(3) 3_655 .
T3SI O9 T3SI 148(3) 2_655 .
T3GE O9 T3GE 148(3) 2_655 .
T1 O10 T2GE 144.0(19) . .
T1 O10 T2SI 144.0(19) . .
T1 O11 T1 143.6(19) 3 .
T1 O12 T1 137.3(19) . 2
T1 O13 Ge1 160.2(15) . .
Ge1 O14 Ge1 117.9(13) 10 .
O13 T1 O10 116.2(14) . .
O13 T1 O11 109.4(12) . .
O10 T1 O11 106.1(12) . .
O13 T1 O12 104.4(12) . .
O10 T1 O12 109.3(11) . .
O11 T1 O12 111.5(12) . .
O7 T2SI O7 114(2) 4 .
O7 T2SI O10 107.8(15) 4 4
O7 T2SI O10 108.7(15) . 4
O7 T2SI O10 108.7(15) 4 .
O7 T2SI O10 107.8(15) . .
O10 T2SI O10 109.9(19) 4 .
O9 T3SI O8 106.9(17) . .
O9 T3SI O7 106.6(12) . .
O8 T3SI O7 107.0(11) . .
O9 T3SI O2 120.7(15) . 8
O8 T3SI O2 108.1(15) . 8
O7 T3SI O2 106.9(13) . 8
O7 T2GE O7 114(2) 4 .
O7 T2GE O10 107.8(15) 4 4
O7 T2GE O10 108.7(15) . 4
O7 T2GE O10 108.7(15) 4 .
O7 T2GE O10 107.8(15) . .
O10 T2GE O10 109.9(19) 4 .
O9 T3GE O8 106.9(17) . .
O9 T3GE O7 106.6(12) . .
O8 T3GE O7 107.0(11) . .
O9 T3GE O2 120.7(15) . 8
O8 T3GE O2 108.1(15) . 8
O7 T3GE O2 106.9(13) . 8
O6 Ge1 O4 114.9(8) . .
O6 Ge1 O14 111.6(9) . .
O4 Ge1 O14 111.4(10) . .
O6 Ge1 O13 109.5(9) . .
O4 Ge1 O13 105.9(9) . .
O14 Ge1 O13 102.7(9) . .
O5 Ge2 O5 180.0 . 13
O5 Ge2 O6 88.5(7) . 10
O5 Ge2 O6 91.5(7) 13 10
O5 Ge2 O6 91.5(7) . 6
O5 Ge2 O6 88.5(7) 13 6
O6 Ge2 O6 180.0(10) 10 6
O5 Ge2 O6 91.5(7) . 13
O5 Ge2 O6 88.5(7) 13 13
O6 Ge2 O6 89.0(9) 10 13
O6 Ge2 O6 91.0(9) 6 13
O5 Ge2 O6 88.5(7) . .
O5 Ge2 O6 91.5(7) 13 .
O6 Ge2 O6 91.0(9) 10 .
O6 Ge2 O6 89.0(9) 6 .
O6 Ge2 O6 180.0 13 .
O1 Ge3 O4 116.5(8) . .
O1 Ge3 O3 124.4(10) . .
O4 Ge3 O3 118.6(10) . .
O1 Ge3 O2 93.7(8) . .
O4 Ge3 O2 90.9(8) . .
O3 Ge3 O2 92.5(9) . .
O1 Ge3 O5 93.5(9) . .
O4 Ge3 O5 90.6(8) . .
O3 Ge3 O5 79.0(8) . .
O2 Ge3 O5 171.0(8) . .
O1 Ge3 Ge3 114.1(6) . 10
O4 Ge3 Ge3 112.1(5) . 10
O3 Ge3 Ge3 34.9(7) . 10
O2 Ge3 Ge3 127.4(6) . 10
O5 Ge3 Ge3 44.2(5) . 10
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.55(3) .
C2 N1 1.54(3) .
C3 N2 1.50(3) .
C4 N2 1.50(3) .
C5 N2 1.49(3) .
N1 C2 1.54(3) 6_455
N1 C1 1.55(3) 6_455
N2 C4 1.50(3) 10
O1 Ge3 1.751(17) .
O2 T3GE 1.756(18) 8_455
O2 T3SI 1.756(18) 8_455
O2 Ge3 1.823(17) .
O3 Ge3 1.772(14) 10
O3 Ge3 1.772(14) .
O4 Ge1 1.728(17) .
O4 Ge3 1.768(16) .
O5 Ge2 1.87(2) .
O5 Ge3 2.026(16) 10
O5 Ge3 2.026(16) .
O6 Ge1 1.724(17) .
O6 Ge2 1.900(15) .
O7 T2GE 1.63(3) .
O7 T2SI 1.63(3) .
O7 T3GE 1.71(3) .
O7 T3SI 1.71(3) .
O8 T3GE 1.684(13) 3_655
O8 T3SI 1.684(13) 3_655
O8 T3SI 1.684(13) .
O8 T3GE 1.684(13) .
O9 T3GE 1.637(12) 2_655
O9 T3SI 1.637(12) 2_655
O9 T3SI 1.637(12) .
O9 T3GE 1.637(12) .
O10 T1 1.57(3) .
O10 T2GE 1.73(3) .
O10 T2SI 1.73(3) .
O11 T1 1.623(11) 3
O11 T1 1.623(11) .
O12 T1 1.659(12) .
O12 T1 1.660(12) 2
O13 T1 1.545(19) .
O13 Ge1 1.758(17) .
O14 Ge1 1.745(12) 10
O14 Ge1 1.745(12) .
T2SI O7 1.63(3) 4
T2SI O10 1.73(3) 4
T3SI O2 1.756(18) 8
T2GE O7 1.63(3) 4
T2GE O10 1.73(3) 4
T3GE O2 1.756(18) 8
Ge2 O5 1.87(2) 13
Ge2 O6 1.900(15) 10
Ge2 O6 1.900(15) 6
Ge2 O6 1.900(15) 13
Ge3 Ge3 2.906(5) 10
