#------------------------------------------------------------------------------
#$Date: 2016-03-26 19:34:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180440 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/09/7210973.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_7210973
loop_
_publ_author_name
'Zhang, Ming-Dao'
'Qin, Ling'
'Yao, Xiao-Qiang'
'Yang, Qing-Xiang'
'Guo, Zi-Jian'
'Zheng, He-Gen'
_publ_section_title
;
 The synthesis, structure and third-order nonlinear optical effect of a
 new 2D cluster polymer based on a [WS4Cu4]2+ SBU and
 1,2-di(pyridin-4-yl)ethane
;
_journal_issue                   36
_journal_name_full               CrystEngComm
_journal_page_first              7354
_journal_paper_doi               10.1039/c3ce41033a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C24 H24 Cu4 I2 N4 S4 W'
_chemical_formula_sum            'C24 H24 Cu4 I2 N4 S4 W'
_chemical_formula_weight         1188.52
_chemical_name_systematic
;
?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_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                   9.3967(3)
_cell_length_b                   9.3967(3)
_cell_length_c                   32.3703(18)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.374
_cell_measurement_theta_min      2.258
_cell_volume                     2858.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0158
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            15761
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    4.708
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         0.566
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         2510
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0323
_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)+(0.0856P)²+6.9900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1217
_reflns_number_gt                2322
_reflns_number_total             2510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41033a.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P4(2)/n
_cod_database_code               7210973
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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
W1 W 0.2500 0.2500 0.2500 0.02754(15) Uani 1 4 d S
I2 I 0.7500 0.2500 0.296725(16) 0.04658(19) Uani 1 2 d S
Cu1 Cu 0.53281(8) 0.31733(8) 0.24869(2) 0.0418(2) Uani 1 1 d U
S1 S 0.41415(14) 0.14309(13) 0.21129(4) 0.035 Uani 1 1 d U
N1 N 0.6165(5) 0.4411(5) 0.20235(15) 0.0451(11) Uani 1 1 d U
C3 C 0.7283(6) 0.5919(6) 0.13439(18) 0.0429(12) Uani 1 1 d .
C4 C 0.8019(6) 0.5796(6) 0.17182(18) 0.0424(12) Uani 1 1 d .
H4 H 0.8911 0.6214 0.1745 0.051 Uiso 1 1 calc R
C6 C 0.7835(7) 0.6743(7) 0.09844(19) 0.0506(14) Uani 1 1 d .
H6A H 0.7597 0.6256 0.0729 0.061 Uiso 1 1 calc R
H6B H 0.8863 0.6817 0.1002 0.061 Uiso 1 1 calc R
C5 C 0.7446(5) 0.5069(6) 0.20461(18) 0.0406(13) Uani 1 1 d .
H5 H 0.7954 0.5026 0.2292 0.049 Uiso 1 1 calc R
C2 C 0.5957(7) 0.5226(8) 0.1330(2) 0.0614(18) Uani 1 1 d .
H2 H 0.5431 0.5218 0.1086 0.074 Uiso 1 1 calc R
C1 C 0.5452(7) 0.4575(8) 0.1670(2) 0.065(2) Uani 1 1 d U
H1 H 0.4533 0.4210 0.1657 0.078 Uiso 1 1 calc R
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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
W W -0.8490 6.8722 '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
S1 W1 S1 111.51(7) 8_656 7_566
S1 W1 S1 108.46(4) 8_656 .
S1 W1 S1 108.46(4) 7_566 .
S1 W1 S1 108.46(4) 8_656 2
S1 W1 S1 108.46(4) 7_566 2
S1 W1 S1 111.51(7) . 2
S1 W1 Cu1 53.81(4) 8_656 .
S1 W1 Cu1 127.44(4) 7_566 .
S1 W1 Cu1 54.69(4) . .
S1 W1 Cu1 124.09(4) 2 .
S1 W1 Cu1 54.69(4) 8_656 8_656
S1 W1 Cu1 124.09(4) 7_566 8_656
S1 W1 Cu1 127.44(4) . 8_656
S1 W1 Cu1 53.81(4) 2 8_656
Cu1 W1 Cu1 90.0 . 8_656
S1 W1 Cu1 127.44(4) 8_656 2
S1 W1 Cu1 53.81(4) 7_566 2
S1 W1 Cu1 124.09(4) . 2
S1 W1 Cu1 54.69(4) 2 2
Cu1 W1 Cu1 178.21(3) . 2
Cu1 W1 Cu1 90.0 8_656 2
S1 W1 Cu1 124.09(4) 8_656 7_566
S1 W1 Cu1 54.69(4) 7_566 7_566
S1 W1 Cu1 53.81(4) . 7_566
S1 W1 Cu1 127.44(4) 2 7_566
Cu1 W1 Cu1 90.0 . 7_566
Cu1 W1 Cu1 178.21(3) 8_656 7_566
Cu1 W1 Cu1 90.0 2 7_566
Cu1 I2 Cu1 107.91(4) . 2_655
N1 Cu1 S1 117.69(15) . 8_656
N1 Cu1 S1 101.68(15) . .
S1 Cu1 S1 103.22(6) 8_656 .
N1 Cu1 I2 105.63(14) . .
S1 Cu1 I2 108.65(4) 8_656 .
S1 Cu1 I2 120.59(5) . .
N1 Cu1 W1 120.99(14) . .
S1 Cu1 W1 51.74(3) 8_656 .
S1 Cu1 W1 51.51(3) . .
I2 Cu1 W1 133.36(3) . .
W1 S1 Cu1 74.45(4) . 7_566
W1 S1 Cu1 73.81(4) . .
Cu1 S1 Cu1 113.90(6) 7_566 .
C1 N1 C5 116.0(5) . .
C1 N1 Cu1 120.0(4) . .
C5 N1 Cu1 124.0(4) . .
C4 C3 C2 115.3(5) . .
C4 C3 C6 123.1(5) . .
C2 C3 C6 121.6(6) . .
C5 C4 C3 121.1(5) . .
C5 C4 H4 119.5 . .
C3 C4 H4 119.5 . .
C3 C6 C6 109.5(5) . 2_665
C3 C6 H6A 109.8 . .
C6 C6 H6A 109.8 2_665 .
C3 C6 H6B 109.8 . .
C6 C6 H6B 109.8 2_665 .
H6A C6 H6B 108.2 . .
N1 C5 C4 122.3(5) . .
N1 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
C1 C2 C3 119.8(6) . .
C1 C2 H2 120.1 . .
C3 C2 H2 120.1 . .
N1 C1 C2 125.2(6) . .
N1 C1 H1 117.4 . .
C2 C1 H1 117.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 S1 2.2268(12) 8_656
W1 S1 2.2268(12) 7_566
W1 S1 2.2268(12) .
W1 S1 2.2268(12) 2
W1 Cu1 2.7321(7) .
W1 Cu1 2.7321(7) 8_656
W1 Cu1 2.7321(7) 2
W1 Cu1 2.7321(7) 7_566
I2 Cu1 2.6427(8) .
I2 Cu1 2.6427(8) 2_655
Cu1 N1 2.054(5) .
Cu1 S1 2.2888(15) 8_656
Cu1 S1 2.3214(14) .
S1 Cu1 2.2888(15) 7_566
N1 C1 1.336(8) .
N1 C5 1.355(7) .
C3 C4 1.400(8) .
C3 C2 1.407(9) .
C3 C6 1.491(8) .
C4 C5 1.373(8) .
C4 H4 0.9300 .
C6 C6 1.555(13) 2_665
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C5 H5 0.9300 .
C2 C1 1.345(10) .
C2 H2 0.9300 .
C1 H1 0.9300 .
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 -0.021 -0.007 0.000 739 326 ' '
2 -0.023 0.193 0.500 739 324 ' '
