#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:24:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179842 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/38/7013811.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_7013811
loop_
_publ_author_name
'Villaescusa, Luis A.'
'Wheatley, Paul S.'
'Morris, Russell E.'
'Lightfoot, Philip'
_publ_section_title
;
 A severely interrupted germanate zeolite framework synthesised from
 isolated double four-ring units.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              820
_journal_page_last               824
_journal_paper_doi               10.1039/b314942k
_journal_year                    2004
_chemical_formula_sum            'F3 Ge25.5 O53'
_chemical_formula_weight         2756.0
_chemical_name_systematic
;
?
;
_space_group_IT_number           63
_symmetry_cell_setting           Cmcm
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.081(2)
_cell_length_b                   18.5854(13)
_cell_length_c                   13.9571(10)
_cell_measurement_temperature    293(2)
_cell_volume                     8581.2(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6899
_diffrn_reflns_av_R_equivalents  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25017
_diffrn_reflns_theta_full        30.40
_diffrn_reflns_theta_max         30.40
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    9.043
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5068
_refine_diff_density_max         7.418
_refine_diff_density_min         -4.675
_refine_diff_density_rms         0.542
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.303
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         6308
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.1031
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1036P)²+447.2657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2693
_refine_ls_wR_factor_ref         0.2744
_reflns_number_gt                5577
_reflns_number_total             6308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b314942k.txt
_cod_data_source_block           STAG-1
_cod_original_cell_volume        8581.3(11)
_cod_database_code               7013811
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, -z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y, z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'-x+1/2, y+1/2, z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.21442(3) 0.12932(5) 0.63467(7) 0.0147(2) Uani 1 1 d . . .
Ge2 Ge 0.28681(3) 0.24066(6) 0.64049(7) 0.0152(2) Uani 1 1 d . . .
Ge3 Ge 0.22612(3) 0.37203(5) 0.63480(7) 0.0146(2) Uani 1 1 d . . .
Ge4 Ge 0.25869(6) 0.5000 0.5000 0.0209(4) Uani 1 2 d S . .
Ge5 Ge 0.15957(3) 0.26243(7) 0.55430(8) 0.0190(3) Uani 1 1 d . . .
O1 O 0.3132(3) 0.2429(6) 0.7500 0.018(2) Uani 1 2 d S . .
O2 O 0.1705(2) 0.2660(5) 0.4332(6) 0.0267(18) Uani 1 1 d . . .
O3 O 0.2624(2) 0.1619(4) 0.6082(6) 0.0227(16) Uani 1 1 d . . .
O4 O 0.2091(5) 0.0966(6) 0.7500 0.031(3) Uani 1 2 d S . .
O5 O 0.1791(2) 0.3345(5) 0.6181(6) 0.0269(17) Uani 1 1 d . . .
O6 O 0.2924(3) 0.4475(5) 0.4342(6) 0.030(2) Uani 1 1 d . . .
O7 O 0.2664(2) 0.3204(4) 0.5951(6) 0.0247(17) Uani 1 1 d . . .
O8 O 0.1730(2) 0.1825(4) 0.6077(6) 0.0257(17) Uani 1 1 d . . .
O9 O 0.2308(5) 0.4034(6) 0.7500 0.031(3) Uani 1 2 d S . .
O10 O 0.2252(3) 0.4518(5) 0.5688(6) 0.031(2) Uani 1 1 d . . .
O11 O 0.1080(2) 0.2702(7) 0.5568(6) 0.040(2) Uani 1 1 d D . .
F1 F 0.2369(3) 0.2482(6) 0.7500 0.043(3) Uani 1 2 d S . .
Ge6 Ge 0.06920(4) 0.26069(10) 0.63922(9) 0.0356(4) Uani 1 1 d D . .
Ge9 Ge 0.0000 0.14582(15) 0.6410(2) 0.0485(6) Uani 1 2 d SD . .
O18 O 0.0452(4) 0.1819(8) 0.6028(11) 0.068(4) Uani 1 1 d . . .
O19 O 0.0000 0.0705(9) 0.5684(17) 0.083(7) Uani 1 2 d SD . .
O20 O 0.0000 0.102(2) 0.7500 0.114(14) Uani 1 4 d S . .
O15 O 0.0000 0.4229(10) 0.7500 0.042(5) Uani 1 4 d S . .
Ge8 Ge 0.0000 0.3888(2) 0.6370(3) 0.0382(12) Uani 0.573(9) 2 d SPD . 1
O16 O 0.0455(5) 0.3438(9) 0.6212(18) 0.060(5) Uiso 0.573(9) 1 d PD . 1
O13 O 0.0867(5) 0.2875(8) 0.7500 0.0125(19) Uiso 0.573(9) 2 d SPD . 1
F14 F 0.0000 0.2608(19) 0.7500 0.048(6) Uiso 0.573(9) 4 d SP . 1
O17 O 0.0000 0.4942(9) 0.5408(12) 0.0125(19) Uiso 0.573(9) 2 d SP . 1
Ge7 Ge 0.0000 0.3257(3) 0.7500 0.0182(14) Uani 0.466(11) 4 d SP . 2
O12 O 0.0388(9) 0.3243(17) 0.657(2) 0.060(5) Uiso 0.466(11) 1 d P . 2
O13A O 0.0933(6) 0.2332(11) 0.7500 0.0125(19) Uiso 0.466(11) 2 d SP . 2
F14A F 0.0000 0.213(2) 0.7500 0.048(6) Uiso 0.466(11) 4 d SP . 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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
_geom_angle_publ_flag
O4 Ge1 O8 108.8(6) . . ?
O4 Ge1 O3 114.4(6) . . ?
O8 Ge1 O3 118.6(4) . . ?
O4 Ge1 O6 102.3(4) . 13_556 ?
O8 Ge1 O6 104.2(5) . 13_556 ?
O3 Ge1 O6 106.7(4) . 13_556 ?
O3 Ge2 O7 116.3(4) . . ?
O3 Ge2 O2 99.4(4) . 13_556 ?
O7 Ge2 O2 99.1(4) . 13_556 ?
O3 Ge2 O1 118.5(5) . . ?
O7 Ge2 O1 119.1(5) . . ?
O2 Ge2 O1 96.4(4) 13_556 . ?
O3 Ge2 F1 83.6(4) . . ?
O7 Ge2 F1 84.8(3) . . ?
O2 Ge2 F1 173.2(3) 13_556 . ?
O1 Ge2 F1 76.9(3) . . ?
O9 Ge3 O5 110.3(6) . . ?
O9 Ge3 O7 114.7(6) . . ?
O5 Ge3 O7 115.3(4) . . ?
O9 Ge3 O10 102.0(5) . . ?
O5 Ge3 O10 104.9(5) . . ?
O7 Ge3 O10 108.3(4) . . ?
O10 Ge4 O10 99.8(6) 3_566 . ?
O10 Ge4 O6 114.5(4) 3_566 3_566 ?
O10 Ge4 O6 114.2(5) . 3_566 ?
O10 Ge4 O6 114.2(5) 3_566 . ?
O10 Ge4 O6 114.5(4) . . ?
O6 Ge4 O6 100.4(6) 3_566 . ?
O11 Ge5 O8 108.7(5) . . ?
O11 Ge5 O2 103.0(4) . . ?
O8 Ge5 O2 113.8(4) . . ?
O11 Ge5 O5 107.2(5) . . ?
O8 Ge5 O5 110.4(4) . . ?
O2 Ge5 O5 113.2(4) . . ?
Ge2 O1 Ge2 120.4(6) . 10_557 ?
Ge5 O2 Ge2 137.7(5) . 13_556 ?
Ge2 O3 Ge1 131.7(4) . . ?
Ge1 O4 Ge1 137.1(7) 10_557 . ?
Ge3 O5 Ge5 136.1(5) . . ?
Ge1 O6 Ge4 131.9(6) 13_556 . ?
Ge3 O7 Ge2 130.6(4) . . ?
Ge5 O8 Ge1 142.3(5) . . ?
Ge3 O9 Ge3 138.9(7) . 10_557 ?
Ge4 O10 Ge3 136.7(5) . . ?
Ge5 O11 Ge6 137.9(5) . . ?
Ge2 F1 Ge2 85.4(3) 10_557 . ?
O12 Ge6 O18 112.8(13) . . ?
O12 Ge6 O11 120.3(12) . . ?
O18 Ge6 O11 103.2(6) . . ?
O12 Ge6 O13 81.5(13) . . ?
O18 Ge6 O13 131.2(7) . . ?
O11 Ge6 O13 108.5(6) . . ?
O12 Ge6 O16 22.1(12) . . ?
O18 Ge6 O16 119.7(10) . . ?
O11 Ge6 O16 98.4(8) . . ?
O13 Ge6 O16 91.4(10) . . ?
O12 Ge6 O13A 110.8(13) . . ?
O18 Ge6 O13A 102.3(9) . . ?
O11 Ge6 O13A 105.6(6) . . ?
O13 Ge6 O13A 33.8(8) . . ?
O16 Ge6 O13A 124.7(10) . . ?
O18 Ge9 O18 120.4(11) . 11 ?
O18 Ge9 O20 117.1(6) . . ?
O18 Ge9 O20 117.1(6) 11 . ?
O18 Ge9 O19 97.7(6) . . ?
O18 Ge9 O19 97.7(6) 11 . ?
O20 Ge9 O19 97.9(15) . . ?
O18 Ge9 F14A 89.5(7) . . ?
O18 Ge9 F14A 89.5(7) 11 . ?
O20 Ge9 F14A 67.5(16) . . ?
O19 Ge9 F14A 165.4(13) . . ?
Ge9 O18 Ge6 129.2(9) . . ?
Ge9 O20 Ge9 124(2) 10_557 . ?
Ge8 O15 Ge8 136.2(12) 10_557 . ?
Ge8 O15 Ge7 68.1(6) 10_557 . ?
Ge8 O15 Ge7 68.1(6) . . ?
O15 Ge8 O16 107.3(9) . . ?
O15 Ge8 O16 107.3(9) . 11 ?
O16 Ge8 O16 120.2(16) . 11 ?
Ge8 O16 Ge6 142.7(14) . . ?
Ge6 O13 Ge6 127.4(9) . 10_557 ?
O15 Ge7 O12 90.8(10) . 10_557 ?
O15 Ge7 O12 90.8(10) . 4_556 ?
O12 Ge7 O12 90(2) 10_557 4_556 ?
O15 Ge7 O12 90.8(10) . 11 ?
O12 Ge7 O12 178(2) 10_557 11 ?
O12 Ge7 O12 90(2) 4_556 11 ?
O15 Ge7 O12 90.8(10) . . ?
O12 Ge7 O12 90(2) 10_557 . ?
O12 Ge7 O12 178(2) 4_556 . ?
O12 Ge7 O12 90(2) 11 . ?
O15 Ge7 F14A 180.000(8) . . ?
O12 Ge7 F14A 89.2(10) 10_557 . ?
O12 Ge7 F14A 89.2(10) 4_556 . ?
O12 Ge7 F14A 89.2(10) 11 . ?
O12 Ge7 F14A 89.2(10) . . ?
Ge6 O12 Ge7 125.2(19) . . ?
Ge6 O13A Ge6 117.0(11) 10_557 . ?
Ge9 F14A Ge9 101(2) . 10_557 ?
Ge9 F14A Ge7 129.5(10) . . ?
Ge9 F14A Ge7 129.5(10) 10_557 . ?
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
Ge1 O4 1.729(4) . ?
Ge1 O8 1.732(8) . ?
Ge1 O3 1.739(8) . ?
Ge1 O6 1.737(8) 13_556 ?
Ge2 O3 1.731(7) . ?
Ge2 O7 1.748(7) . ?
Ge2 O2 1.751(8) 13_556 ?
Ge2 O1 1.761(5) . ?
Ge2 F1 2.254(7) . ?
Ge3 O9 1.717(4) . ?
Ge3 O5 1.720(8) . ?
Ge3 O7 1.732(7) . ?
Ge3 O10 1.745(8) . ?
Ge4 O10 1.718(8) 3_566 ?
Ge4 O10 1.718(8) . ?
Ge4 O6 1.743(9) 3_566 ?
Ge4 O6 1.743(8) . ?
Ge5 O11 1.713(8) . ?
Ge5 O8 1.720(8) . ?
Ge5 O2 1.730(8) . ?
Ge5 O5 1.734(9) . ?
O1 Ge2 1.761(5) 10_557 ?
O2 Ge2 1.751(8) 13_556 ?
O4 Ge1 1.729(4) 10_557 ?
O6 Ge1 1.737(8) 13_556 ?
O9 Ge3 1.717(4) 10_557 ?
O11 Ge6 1.732(8) . ?
F1 Ge2 2.254(7) 10_557 ?
Ge6 O12 1.57(3) . ?
Ge6 O18 1.741(14) . ?
Ge6 O13 1.725(7) . ?
Ge6 O16 1.751(12) . ?
Ge6 O13A 1.814(11) . ?
Ge9 O18 1.725(13) . ?
Ge9 O18 1.725(13) 11 ?
Ge9 O20 1.722(19) . ?
Ge9 O19 1.727(13) . ?
Ge9 F14A 1.97(3) . ?
O20 Ge9 1.722(19) 10_557 ?
O15 Ge8 1.700(8) 10_557 ?
O15 Ge8 1.700(8) . ?
O15 Ge7 1.81(2) . ?
Ge8 O16 1.734(12) . ?
Ge8 O16 1.734(12) 11 ?
O13 Ge6 1.725(7) 10_557 ?
O17 O17 1.16(3) 9_566 ?
Ge7 O12 1.82(3) 10_557 ?
Ge7 O12 1.82(3) 4_556 ?
Ge7 O12 1.82(3) 11 ?
Ge7 O12 1.82(3) . ?
Ge7 F14A 2.09(5) . ?
O13A Ge6 1.814(11) 10_557 ?
F14A Ge9 1.97(3) 10_557 ?
