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#$Date: 2016-03-21 18:11:13 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178804 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/58/4105841.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_4105841
loop_
_publ_author_name
'Mei-Chun Chen'
'Long-Hua Li'
'Yu-Biao Chen'
'Ling Chen'
_publ_section_title
;
 In-Phase Alignments of Asymmetric Building Units in Ln4GaSbS9 (Ln = Pr,
 Nd, Sm, Gd-Ho) and Their Strong Nonlinear Optical Responses in Middle IR
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4617
_journal_page_last               4624
_journal_paper_doi               10.1021/ja1111095
_journal_volume                  133
_journal_year                    2011
_chemical_formula_sum            'Ga Gd4 S9 Sb'
_chemical_formula_weight         1109.01
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           41
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'A 2 -2ab'
_symmetry_space_group_name_H-M   'A b a 2'
_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            8
_cell_length_a                   13.5733(16)
_cell_length_b                   13.8956(18)
_cell_length_c                   14.0982(19)
_cell_measurement_reflns_used    3972
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4719
_cell_measurement_theta_min      3.0014
_cell_volume                     2659.0(6)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_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  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9588
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    25.034
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4961
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orangeyellow
_exptl_crystal_density_diffrn    5.540
_exptl_crystal_description       block
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.053
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.244
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.032(14)
_refine_ls_extinction_coef       0.00032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.307
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2931
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.307
_refine_ls_R_factor_all          0.0128
_refine_ls_R_factor_gt           0.0114
_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/[σ²(Fo²)+(0.0258P)²+12.9099P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0265
_refine_ls_wR_factor_ref         0.0596
_reflns_number_gt                2817
_reflns_number_total             2931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1111095_si_001_4.cif
_cod_data_source_block           Gd4GaSbS9
_cod_database_code               4105841
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, 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
Gd1 Gd 0.68586(3) 0.60928(3) 0.98165(3) 0.00884(11) Uani 1 1 d .
Gd2 Gd 0.89897(3) 0.82804(3) 0.99231(3) 0.00932(11) Uani 1 1 d .
Gd3 Gd 0.81831(3) 0.83434(3) 0.70873(3) 0.01029(11) Uani 1 1 d .
Gd4 Gd 0.60386(3) 0.88847(3) 0.93892(3) 0.01048(11) Uani 1 1 d .
Sb Sb 0.88728(5) 0.57959(5) 0.75204(5) 0.01449(15) Uani 1 1 d .
Ga Ga 0.59229(7) 0.60516(7) 0.71901(8) 0.0092(2) Uani 1 1 d .
S1 S 0.90056(15) 0.59002(16) 0.92478(17) 0.0098(4) Uani 1 1 d .
S2 S 0.58147(16) 0.90639(16) 0.74046(17) 0.0117(4) Uani 1 1 d .
S3 S 0.69730(16) 0.51148(16) 0.80630(17) 0.0100(4) Uani 1 1 d .
S4 S 0.69005(16) 0.69790(16) 0.62366(16) 0.0086(4) Uani 1 1 d .
S5 S 1.0000 1.0000 0.6288(3) 0.0206(8) Uani 1 2 d S
S6 S 0.99276(17) 0.80523(16) 0.81351(17) 0.0124(4) Uani 1 1 d .
S7 S 0.93227(16) 0.74703(16) 0.56688(16) 0.0083(4) Uani 1 1 d .
S8 S 0.74903(17) 0.94278(15) 0.56142(16) 0.0092(4) Uani 1 1 d .
S9 S 1.0000 1.0000 1.0000(3) 0.0130(7) Uani 1 2 d S
S10 S 0.74586(17) 0.76579(16) 0.87552(16) 0.0091(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Gd Gd -0.1653 3.9035 '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
S8 Gd1 S10 143.43(7) 5_545 .
S8 Gd1 S7 126.34(7) 5_545 8_645
S10 Gd1 S7 82.05(7) . 8_645
S8 Gd1 S3 86.28(7) 5_545 .
S10 Gd1 S3 83.60(7) . .
S7 Gd1 S3 138.03(7) 8_645 .
S7 Gd2 S8 134.45(7) 6_765 8_645
S7 Gd2 S9 84.18(6) 6_765 .
S8 Gd2 S9 81.17(6) 8_645 .
S7 Gd2 S10 137.28(7) 6_765 .
S8 Gd2 S10 81.04(7) 8_645 .
S9 Gd2 S10 131.50(8) . .
S10 Gd3 S8 136.50(7) . .
S10 Gd3 S7 131.62(7) . .
S8 Gd3 S7 83.48(7) . .
S10 Gd3 S6 78.50(7) . .
S8 Gd3 S6 140.01(7) . .
S7 Gd3 S6 81.28(7) . .
S7 Gd4 S10 83.84(7) 8_645 .
S7 Gd4 S8 84.97(7) 8_645 8_645
S10 Gd4 S8 82.18(7) . 8_645
S7 Gd4 S1 86.92(7) 8_645 3_465
S10 Gd4 S1 138.19(7) . 3_465
S8 Gd4 S1 137.45(7) 8_645 3_465
S1 Sb S2 96.42(8) . 4_645
S1 Sb S2 89.06(7) . 3_565
S2 Sb S2 84.02(8) 4_645 3_565
S1 Sb S3 79.59(7) . .
S2 Sb S3 81.28(7) 4_645 .
S2 Sb S3 160.24(7) 3_565 .
S6 Ga S4 112.42(9) 3_465 .
S6 Ga S3 111.53(10) 3_465 .
S4 Ga S3 105.98(8) . .
S6 Ga S5 110.36(8) 3_465 3_465
S4 Ga S5 110.37(10) . 3_465
S3 Ga S5 105.91(8) . 3_465
Sb S1 Gd4 98.67(8) . 3_565
Sb S1 Gd4 90.57(8) . 4_645
Gd4 S1 Gd4 97.08(7) 3_565 4_645
Sb S1 Gd1 101.39(8) . .
Gd4 S1 Gd1 157.51(9) 3_565 .
Gd4 S1 Gd1 92.79(6) 4_645 .
Sb S2 Sb 95.51(8) 4_655 3_465
Sb S2 Gd4 90.11(7) 4_655 .
Sb S2 Gd4 93.01(7) 3_465 .
Ga S3 Gd1 99.36(8) . .
Ga S3 Gd3 100.77(9) . 4_645
Gd1 S3 Gd3 147.17(9) . 4_645
Ga S3 Sb 103.30(9) . .
Gd1 S3 Sb 97.17(7) . .
Gd3 S3 Sb 103.07(7) 4_645 .
Ga S4 Gd3 118.93(9) . .
Ga S4 Gd2 119.50(9) . 8_644
Gd3 S4 Gd2 96.34(7) . 8_644
Ga S4 Gd1 120.34(9) . 8_644
Gd3 S4 Gd1 102.69(7) . 8_644
Gd2 S4 Gd1 93.85(7) 8_644 8_644
Ga S5 Ga 113.10(16) 4_655 3_565
Ga S6 Gd3 96.53(9) 3_565 .
Ga S6 Gd2 136.57(10) 3_565 .
Gd3 S6 Gd2 94.16(7) . .
Gd4 S7 Gd2 99.94(8) 8_644 6_764
Gd4 S7 Gd1 96.17(7) 8_644 8_644
Gd2 S7 Gd1 93.13(7) 6_764 8_644
Gd4 S7 Gd3 93.50(7) 8_644 .
Gd2 S7 Gd3 154.62(9) 6_764 .
Gd1 S7 Gd3 106.79(7) 8_644 .
Gd1 S8 Gd3 153.44(9) 5_554 .
Gd1 S8 Gd2 96.72(7) 5_554 8_644
Gd3 S8 Gd2 101.62(7) . 8_644
Gd1 S8 Gd4 101.75(7) 5_554 8_644
Gd3 S8 Gd4 94.37(7) . 8_644
Gd2 S8 Gd4 98.59(7) 8_644 8_644
Gd2 S9 Gd2 175.49(15) . 2_775
Gd2 S9 Gd1 90.992(17) . 4_655
Gd2 S9 Gd1 88.614(17) 2_775 4_655
Gd2 S9 Gd1 88.614(17) . 3_565
Gd2 S9 Gd1 90.992(17) 2_775 3_565
Gd1 S9 Gd1 169.96(14) 4_655 3_565
Gd3 S10 Gd4 108.68(8) . .
Gd3 S10 Gd1 148.23(9) . .
Gd4 S10 Gd1 96.11(7) . .
Gd3 S10 Gd2 97.60(7) . .
Gd4 S10 Gd2 98.01(7) . .
Gd1 S10 Gd2 98.28(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Gd1 S8 2.712(2) 5_545
Gd1 S10 2.762(2) .
Gd1 S7 2.771(2) 8_645
Gd1 S3 2.825(2) .
Gd2 S7 2.728(2) 6_765
Gd2 S8 2.744(2) 8_645
Gd2 S9 2.7571(5) .
Gd2 S10 2.789(2) .
Gd3 S10 2.721(2) .
Gd3 S8 2.733(2) .
Gd3 S7 2.804(2) .
Gd3 S6 2.820(2) .
Gd4 S7 2.712(2) 8_645
Gd4 S10 2.724(2) .
Gd4 S8 2.746(2) 8_645
Gd4 S1 2.783(2) 3_465
Sb S1 2.446(2) .
Sb S2 2.449(2) 4_645
Sb S2 2.648(2) 3_565
Sb S3 2.851(2) .
Ga S6 2.269(2) 3_465
Ga S4 2.286(2) .
Ga S3 2.289(2) .
Ga S5 2.307(2) 3_465
S1 Gd4 2.783(2) 3_565
S1 Gd4 2.808(2) 4_645
S2 Sb 2.449(2) 4_655
S2 Sb 2.648(2) 3_465
S3 Gd3 2.828(2) 4_645
S4 Gd2 2.857(2) 8_644
S4 Gd1 2.892(2) 8_644
S5 Ga 2.307(2) 4_655
S5 Ga 2.307(2) 3_565
S6 Ga 2.269(2) 3_565
S7 Gd4 2.712(2) 8_644
S7 Gd2 2.728(2) 6_764
S7 Gd1 2.771(2) 8_644
S8 Gd1 2.712(2) 5_554
S8 Gd2 2.744(2) 8_644
S8 Gd4 2.746(2) 8_644
S9 Gd2 2.7571(5) 2_775
S9 Gd1 2.9559(6) 4_655
S9 Gd1 2.9559(6) 3_565
