#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:31:45 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179451 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/48/4334827.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_4334827
loop_
_publ_author_name
'Xiang Xu'
'Chun-Li Hu'
'Fang Kong'
'Jian-Han Zhang'
'Jiang-Gao Mao'
'Junliang Sun'
_publ_section_title
;
 Cs2GeB4O9: a New Second-Order Nonlinear-Optical Crystal
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5831
_journal_page_last               5837
_journal_paper_doi               10.1021/ic302774h
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'B4 Cs2 Ge O9'
_chemical_formula_weight         525.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8063(2)
_cell_length_b                   6.8063(2)
_cell_length_c                   9.9523(7)
_cell_measurement_temperature    293(2)
_cell_volume                     461.05(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 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'SuperNova (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0223
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2447
_diffrn_reflns_theta_full        27.33
_diffrn_reflns_theta_max         27.33
_diffrn_reflns_theta_min         3.63
_exptl_absorpt_coefficient_mu    11.131
_exptl_absorpt_correction_T_max  0.5096
_exptl_absorpt_correction_T_min  0.2690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrystalClear Version 1.3.5. Rigaku Corp., Woodlands, TX, 1999
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.787
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.643
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.120
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(4)
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         516
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0223
_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)+(0.0114P)²+3.1867P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0440
_reflns_number_gt                515
_reflns_number_total             516
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302774h_si_002.cif
_cod_data_source_block           Cs2GeB4O9
_cod_database_code               4334827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+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
Cs1 Cs 0.0000 0.0000 0.0000 0.0406(2) Uani 1 4 d S
Cs2 Cs 0.0000 0.5000 0.2500 0.0309(3) Uani 1 4 d S
Ge1 Ge 0.0000 0.5000 0.7500 0.0146(3) Uani 1 4 d S
B1 B 0.0623(16) 0.1673(15) 0.5822(10) 0.015(2) Uani 0.50 1 d PDU
B2 B 0.0845(17) 0.2213(17) 0.5560(12) 0.015(2) Uani 0.50 1 d PD
O1 O 0.1453(5) 0.3393(5) 0.6570(3) 0.0191(7) Uani 1 1 d D
O2 O 0.2272(4) 0.1047(4) 0.4955(8) 0.0230(7) Uani 1 1 d D
O3 O 0.0000 0.0000 0.6616(6) 0.0131(13) Uani 0.50 2 d SPD
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cs1 0.0319(2) 0.0319(2) 0.0579(5) 0.000 0.000 0.000
Cs2 0.0348(5) 0.0348(5) 0.0231(5) 0.000 0.000 0.000
Ge1 0.0165(5) 0.0165(5) 0.0108(6) 0.000 0.000 0.000
B1 0.021(3) 0.018(5) 0.005(4) 0.001(3) 0.000(3) 0.005(3)
B2 0.021(3) 0.018(5) 0.005(4) 0.001(3) 0.000(3) 0.005(3)
O1 0.0123(16) 0.0267(19) 0.0184(17) -0.0055(14) 0.0007(13) 0.0036(13)
O2 0.0183(13) 0.0174(13) 0.0333(18) 0.005(3) 0.008(3) 0.0005(10)
O3 0.019(9) 0.008(8) 0.013(3) 0.000 0.000 -0.004(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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'
O O 0.0106 0.0060 '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
O1 Ge1 O1 106.41(10) 8_556 .
O1 Ge1 O1 106.41(10) 8_556 2_565
O1 Ge1 O1 115.8(2) . 2_565
O1 Ge1 O1 115.8(2) 8_556 7_456
O1 Ge1 O1 106.41(10) . 7_456
O1 Ge1 O1 106.41(10) 2_565 7_456
O2 B1 O3 106.6(7) 4_556 .
O2 B1 O2 111.6(7) 4_556 .
O3 B1 O2 108.3(7) . .
O2 B1 O1 110.2(7) 4_556 .
O3 B1 O1 117.0(7) . .
O2 B1 O1 103.2(7) . .
O1 B2 O2 122.8(9) . 4_556
O1 B2 O2 116.5(8) . .
O2 B2 O2 120.4(8) 4_556 .
B2 O1 B1 18.3(7) . .
B2 O1 Ge1 126.5(5) . .
B1 O1 Ge1 122.8(5) . .
B2 O2 B2 132.0(9) 3_556 .
B2 O2 B1 19.3(7) 3_556 3_556
B2 O2 B1 119.1(6) . 3_556
B2 O2 B1 117.5(6) 3_556 .
B2 O2 B1 18.8(6) . .
B1 O2 B1 109.1(8) 3_556 .
B1 O3 B1 113.9(10) 2 .
B1 O3 B2 0.4(7) 2 2
B1 O3 B2 113.8(5) . 2
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 O1 1.741(3) 8_556
Ge1 O1 1.741(3) .
Ge1 O1 1.741(3) 2_565
Ge1 O1 1.741(3) 7_456
B1 O2 1.434(11) 4_556
B1 O3 1.450(10) .
B1 O2 1.479(11) .
B1 O1 1.498(11) .
B2 O1 1.352(11) .
B2 O2 1.386(11) 4_556
B2 O2 1.392(11) .
O2 B2 1.386(11) 3_556
O2 B1 1.434(11) 3_556
O3 B1 1.450(10) 2
O3 B2 1.925(13) 2
