New Second-Order NLO Materials Based on Polymeric Borate Clusters and GeO4 Tetrahedra: A Combined Experimental and Theoretical Study
Jian-Han Zhang; Chun-Li Hu; Xiang Xu; Fang Kong; Jiang-Gao Mao; Inorganic Chemistry 50 (2011) 1973–1982; doi:10.1021/ic102451n

data_4324557
_publ_section_title
;
 New Second-Order NLO Materials Based on Polymeric Borate Clusters and
 GeO4 Tetrahedra: A Combined Experimental and Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1973
_journal_page_last               1982
_journal_paper_doi               10.1021/ic102451n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'B6 Ge3 O17 Rb4'
_chemical_formula_weight         896.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 103.723(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.845(4)
_cell_length_b                   6.9682(19)
_cell_length_c                   20.253(7)
_cell_measurement_reflns_used    2385
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.1060
_cell_volume                     1623.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Saturn70 (4x4 bin mode)'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0243
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            4601
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    17.521
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4593
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    3.667
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.282(9)
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         1898
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0152
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0355
_reflns_number_gt                1837
_reflns_number_total             1898
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102451n_si_002_3.cif
_cod_data_source_block           Rb4Ge3B6O17
_cod_original_cell_volume        1624.0(9)
_cod_database_code               4324557