Functionalization Based on the Substitutional Flexibility: Strong Middle IR Nonlinear Optical Selenides AXII4XIII5Se12
Hua Lin; Ling Chen; Liu-Jiang Zhou; Li-Ming Wu; Journal of the American Chemical Society 135 (2013) 12914–12921; doi:10.1021/ja4074084

data_4120425
_publ_section_title
;
 Functionalization Based on the Substitutional Flexibility: Strong Middle
 IR Nonlinear Optical Selenides AXII4XIII5Se12
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12914
_journal_page_last               12921
_journal_paper_doi               10.1021/ja4074084
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'Cd4 Cs Ga5 Se12'
_chemical_formula_sum            'Cd4 Cs Ga5 Se12'
_chemical_formula_weight         1878.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.4204(8)
_cell_length_b                   14.4204(8)
_cell_length_c                   9.7803(13)
_cell_measurement_reflns_used    1609
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4547
_cell_measurement_theta_min      2.6453
_cell_volume                     1761.3(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 14.6306
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  Mercury70
_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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4626
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.65
_exptl_absorpt_coefficient_mu    29.300
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7689
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange-red
_exptl_crystal_density_diffrn    5.313
_exptl_crystal_description       Block
_exptl_crystal_F_000             2430
_exptl_crystal_size_max          0.1200
_exptl_crystal_size_mid          0.1100
_exptl_crystal_size_min          0.1100
_refine_diff_density_max         1.674
_refine_diff_density_min         -1.878
_refine_diff_density_rms         0.230
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_coef       0.00144(4)
_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   1.012
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1671
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0729
_reflns_number_gt                1546
_reflns_number_total             1671
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4074084_si_002_3.cif
_cod_data_source_block           CsCd4Ga5Se12
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4120425