#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/37/4503700.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_4503700
loop_
_publ_author_name
'Shi, Lei'
'Bonneau, Charlotte'
'Li, Yafeng'
'Sun, Junliang'
'Yue, Huijuan'
'Zou, Xiaodong'
_publ_section_title
;
 SU-22 and SU-23: Layered Germanates Built from 4-Coordinated Ge7Clusters
 Exhibiting Structural Variations on the 44Topology
;
_journal_issue                   10
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3695
_journal_paper_doi               10.1021/cg800304r
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C6 H26.5 F Ge7 N4.5 O17'
_chemical_formula_weight         960.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.151(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0583(8)
_cell_length_b                   16.4484(10)
_cell_length_c                   17.7788(8)
_cell_measurement_temperature    293(2)
_cell_volume                     4648.5(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0714
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14487
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    9.024
_exptl_absorpt_correction_T_max  0.9313
_exptl_absorpt_correction_T_min  0.4051
_exptl_absorpt_correction_type   numerical
_exptl_crystal_density_diffrn    2.746
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3704
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         1.867
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4248
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0430
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0560P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                2892
_reflns_number_total             4248
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800304r_si_001.cif
_cod_data_source_block           fprofit2after
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C6 H26.50 F Ge7 N4.50 O17'
_cod_database_code               4503700
loop_
_symmetry_equiv_pos_as_xyz
'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, -y, -z'
'x, -y, 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
Ge1 Ge 0.73191(5) 0.38321(5) 0.69675(5) 0.0167(2) Uani 1 1 d .
Ge2 Ge 0.86298(5) 0.27955(5) 0.84848(5) 0.0205(2) Uani 1 1 d .
Ge3 Ge 0.71650(6) 0.35387(5) 0.90354(5) 0.0202(2) Uani 1 1 d .
Ge4 Ge 0.60246(5) 0.27834(5) 0.76530(5) 0.0178(2) Uani 1 1 d .
Ge5 Ge 0.75590(5) 0.19893(5) 0.71385(5) 0.0174(2) Uani 1 1 d .
Ge6 Ge 0.90970(5) 0.43537(5) 0.77224(5) 0.0188(2) Uani 1 1 d .
Ge7 Ge 0.74242(5) 0.01239(5) 0.67649(5) 0.0170(2) Uani 1 1 d .
F F 0.7022(3) 0.4226(3) 0.6015(3) 0.0285(12) Uani 1 1 d .
O1 O 0.7679(3) 0.3456(3) 0.7996(3) 0.0202(13) Uani 1 1 d .
O2 O 0.6211(3) 0.3523(3) 0.7017(3) 0.0209(13) Uani 1 1 d .
O3 O 0.7563(3) 0.2826(3) 0.6560(3) 0.0191(13) Uani 1 1 d .
O4 O 0.8425(3) 0.4159(3) 0.6893(3) 0.0204(13) Uani 1 1 d .
O5 O 0.7907(3) -0.0130(3) 0.7659(3) 0.0237(14) Uani 1 1 d .
O6 O 0.8409(4) 0.1956(3) 0.7873(3) 0.0218(13) Uani 1 1 d .
O7 O 0.9410(3) 0.3481(3) 0.8256(3) 0.0244(14) Uani 1 1 d .
O8 O 0.8083(4) 0.2932(3) 0.9274(3) 0.0261(14) Uani 1 1 d .
O9 O 0.7776(4) -0.0381(3) 0.6016(3) 0.0215(13) Uani 1 1 d .
O10 O 0.6219(4) 0.3092(4) 0.8600(3) 0.0267(14) Uani 1 1 d .
O11 O 0.6635(3) 0.1897(3) 0.7558(3) 0.0204(13) Uani 1 1 d .
O12 O 0.6331(3) 0.0053(3) 0.6694(3) 0.0253(14) Uani 1 1 d .
O13 O 0.9428(3) 0.2199(3) 0.9051(3) 0.0184(13) Uani 1 1 d .
O14 O 0.6892(4) 0.3565(4) 0.9986(3) 0.0314(16) Uani 1 1 d .
O15 O 0.7656(3) 0.1143(3) 0.6572(3) 0.0202(13) Uani 1 1 d .
O16 O 0.5000 0.2426(5) 0.7500 0.026(2) Uani 1 2 d S
O17 O 1.0000 0.4818(5) 0.7500 0.024(2) Uani 1 2 d S
O1W O 0.6321(7) 0.3642(6) 0.4593(5) 0.091(3) Uiso 1 1 d .
N2 N 0.5142(5) 0.1117(5) 0.5390(5) 0.042(2) Uiso 1 1 d .
C3 C 0.5717(7) 0.1795(7) 0.5554(6) 0.046(3) Uiso 1 1 d .
C4 C 0.6391(7) 0.1733(7) 0.5030(6) 0.044(3) Uiso 1 1 d .
N3 N 0.6002(5) 0.1937(5) 0.4240(4) 0.0326(19) Uiso 1 1 d .
C2 C 0.4401(7) 0.1251(7) 0.5810(6) 0.045(3) Uiso 1 1 d .
C1 C 0.3813(7) 0.0532(6) 0.5668(6) 0.042(3) Uiso 1 1 d .
N1 N 0.3064(5) 0.0707(5) 0.6051(4) 0.036(2) Uiso 1 1 d .
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'
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'
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
F Ge1 O2 90.9(2) . .
F Ge1 O3 89.8(2) . .
O2 Ge1 O3 91.8(2) . .
F Ge1 O4 87.6(2) . .
O2 Ge1 O4 178.4(2) . .
O3 Ge1 O4 88.5(2) . .
F Ge1 O5 88.1(2) . 4_656
O2 Ge1 O5 89.9(2) . 4_656
O3 Ge1 O5 177.4(3) . 4_656
O4 Ge1 O5 89.8(2) . 4_656
F Ge1 O1 177.0(2) . .
O2 Ge1 O1 91.6(2) . .
O3 Ge1 O1 91.9(2) . .
O4 Ge1 O1 90.0(2) . .
O5 Ge1 O1 90.2(2) 4_656 .
O6 Ge2 O7 116.3(3) . .
O6 Ge2 O8 120.6(3) . .
O7 Ge2 O8 123.1(3) . .
O6 Ge2 O13 89.0(2) . .
O7 Ge2 O13 90.3(2) . .
O8 Ge2 O13 91.1(3) . .
O6 Ge2 O1 94.8(2) . .
O7 Ge2 O1 94.4(2) . .
O8 Ge2 O1 80.8(2) . .
O13 Ge2 O1 171.9(3) . .
O6 Ge2 Ge3 115.51(19) . .
O7 Ge2 Ge3 115.88(19) . .
O8 Ge2 Ge3 34.29(18) . .
O13 Ge2 Ge3 125.40(19) . .
O1 Ge2 Ge3 46.50(17) . .
O10 Ge3 O8 120.2(3) . .
O10 Ge3 O9 116.2(3) . 4_656
O8 Ge3 O9 121.5(3) . 4_656
O10 Ge3 O14 96.4(3) . .
O8 Ge3 O14 95.3(3) . .
O9 Ge3 O14 92.7(3) 4_656 .
O10 Ge3 O1 90.5(2) . .
O8 Ge3 O1 76.2(2) . .
O9 Ge3 O1 89.3(2) 4_656 .
O14 Ge3 O1 171.1(3) . .
O10 Ge3 Ge2 111.13(19) . .
O8 Ge3 Ge2 34.09(19) . .
O9 Ge3 Ge2 110.26(19) 4_656 .
O14 Ge3 Ge2 129.3(2) . .
O1 Ge3 Ge2 42.15(15) . .
O2 Ge4 O16 112.8(2) . .
O2 Ge4 O10 113.9(3) . .
O16 Ge4 O10 106.7(2) . .
O2 Ge4 O11 111.6(3) . .
O16 Ge4 O11 103.4(3) . .
O10 Ge4 O11 107.7(3) . .
O3 Ge5 O15 106.6(3) . .
O3 Ge5 O6 113.8(3) . .
O15 Ge5 O6 106.4(3) . .
O3 Ge5 O11 113.4(3) . .
O15 Ge5 O11 109.1(3) . .
O6 Ge5 O11 107.2(3) . .
O4 Ge6 O17 109.13(19) . .
O4 Ge6 O12 112.1(3) . 4_656
O17 Ge6 O12 104.9(3) . 4_656
O4 Ge6 O7 113.9(3) . .
O17 Ge6 O7 107.4(3) . .
O12 Ge6 O7 108.9(3) 4_656 .
O5 Ge7 O9 116.2(3) . .
O5 Ge7 O12 111.6(3) . .
O9 Ge7 O12 110.3(3) . .
O5 Ge7 O15 109.4(3) . .
O9 Ge7 O15 101.9(3) . .
O12 Ge7 O15 106.7(3) . .
Ge1 O1 Ge2 134.4(3) . .
Ge1 O1 Ge3 134.2(3) . .
Ge2 O1 Ge3 91.3(2) . .
Ge4 O2 Ge1 118.8(3) . .
Ge5 O3 Ge1 117.2(3) . .
Ge6 O4 Ge1 118.3(3) . .
Ge7 O5 Ge1 117.5(3) . 4_646
Ge5 O6 Ge2 120.2(3) . .
Ge6 O7 Ge2 119.1(3) . .
Ge2 O8 Ge3 111.6(3) . .
Ge7 O9 Ge3 123.0(3) . 4_646
Ge4 O10 Ge3 124.8(3) . .
Ge5 O11 Ge4 118.7(3) . .
Ge7 O12 Ge6 118.4(3) . 4_646
Ge5 O15 Ge7 127.6(3) . .
Ge4 O16 Ge4 140.3(5) 2_656 .
Ge6 O17 Ge6 127.7(4) . 2_756
C3 N2 C2 108.2(8) . .
N2 C3 C4 108.1(9) . .
N3 C4 C3 108.7(8) . .
C1 C2 N2 108.7(9) . .
N1 C1 C2 107.3(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 F 1.813(5) .
Ge1 O2 1.865(6) .
Ge1 O3 1.871(5) .
Ge1 O4 1.879(6) .
Ge1 O5 1.886(6) 4_656
Ge1 O1 1.939(5) .
Ge2 O6 1.762(5) .
Ge2 O7 1.774(6) .
Ge2 O8 1.772(6) .
Ge2 O13 1.803(5) .
Ge2 O1 1.973(5) .
Ge2 Ge3 2.9391(13) .
Ge3 O10 1.764(6) .
Ge3 O8 1.781(6) .
Ge3 O9 1.782(5) 4_656
Ge3 O14 1.806(6) .
Ge3 O1 2.133(6) .
Ge4 O2 1.715(5) .
Ge4 O16 1.732(3) .
Ge4 O10 1.744(6) .
Ge4 O11 1.778(5) .
Ge5 O3 1.718(5) .
Ge5 O15 1.739(5) .
Ge5 O6 1.751(6) .
Ge5 O11 1.759(6) .
Ge6 O4 1.729(5) .
Ge6 O17 1.734(3) .
Ge6 O12 1.754(6) 4_656
Ge6 O7 1.755(5) .
Ge7 O5 1.718(6) .
Ge7 O9 1.730(6) .
Ge7 O12 1.746(6) .
Ge7 O15 1.761(5) .
O5 Ge1 1.886(6) 4_646
O9 Ge3 1.782(5) 4_646
O12 Ge6 1.754(6) 4_646
O16 Ge4 1.732(3) 2_656
O17 Ge6 1.734(3) 2_756
N2 C3 1.451(13) .
N2 C2 1.508(14) .
C3 C4 1.528(15) .
C4 N3 1.492(13) .
C2 C1 1.513(15) .
C1 N1 1.492(13) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.007 337 13 ' '
2 0.500 0.500 0.399 337 13 ' '
