#------------------------------------------------------------------------------
#$Date: 2019-11-22 22:38:28 +0200 (Fri, 22 Nov 2019) $
#$Revision: 231458 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/32/4003242.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_4003242
loop_
_publ_author_name
'Ogiwara, Naoki'
'Inukai, Munehiro'
'Itakura, Tomoya'
'Horike, Satoshi'
'Kitagawa, Susumu'
_publ_section_title
;
 Fast Conduction of Organic Cations in Metal Sulfate Frameworks
;
_journal_issue                   11
_journal_name_full               'Chemistry of Materials'
_journal_page_first              3968
_journal_paper_doi               10.1021/acs.chemmater.6b01284
_journal_volume                  28
_journal_year                    2016
_chemical_formula_moiety         'O8 S2 Zn, 2(C6 H11 N2)'
_chemical_formula_sum            'C12 H22 N4 O8 S2 Zn'
_chemical_formula_weight         479.83
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_symmetry_cell_setting           tetragonal
_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            4
_cell_length_a                   14.489(8)
_cell_length_b                   14.489(8)
_cell_length_c                   9.173(5)
_cell_measurement_reflns_used    4747
_cell_measurement_temperature    433(2)
_cell_measurement_theta_max      27.4971
_cell_measurement_theta_min      3.1439
_cell_volume                     1925.7(18)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      433(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Saturn724+ (4x4 bin mode)'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0414
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14891
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.58
_exptl_absorpt_coefficient_mu    1.540
_exptl_absorpt_correction_T_max  0.7482
_exptl_absorpt_correction_T_min  0.7482
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0472
_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)+(0.0503P)²+0.4018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                1697
_reflns_number_total             2208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1_160deC.cif
_cod_data_source_block           ydkr
_cod_original_cell_volume        1925.7(19)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               4003242
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
Zn1 Zn 0.2500 0.7500 0.14116(5) 0.03538(18) Uani 1 2 d S
S1 S 0.28867(5) 0.61330(5) -0.10727(9) 0.0352(2) Uani 1 1 d .
O4 O 0.23451(17) 0.63895(14) 0.0236(3) 0.0534(6) Uani 1 1 d .
O6 O 0.2976(2) 0.51423(16) -0.1094(3) 0.0627(7) Uani 1 1 d .
O5 O 0.37594(16) 0.66164(19) -0.1084(3) 0.0613(7) Uani 1 1 d .
N2 N -0.0085(2) 0.56144(19) -0.1973(4) 0.0569(8) Uani 1 1 d .
N3 N -0.0599(2) 0.6569(2) -0.0397(4) 0.0645(9) Uani 1 1 d .
C10 C 0.0502(3) 0.5194(3) -0.3081(6) 0.0874(15) Uani 1 1 d .
H1 H 0.0563 0.5608 -0.3893 0.131 Uiso 1 1 calc R
H2 H 0.0230 0.4626 -0.3404 0.131 Uiso 1 1 calc R
H3 H 0.1101 0.5072 -0.2675 0.131 Uiso 1 1 calc R
C7 C -0.0869(3) 0.5240(3) -0.1407(5) 0.0673(12) Uani 1 1 d .
H9 H -0.1125 0.4672 -0.1654 0.081 Uiso 1 1 calc R
C11 C -0.0680(4) 0.7409(4) 0.0482(7) 0.0975(16) Uani 1 1 d .
H7 H -0.0936 0.7254 0.1427 0.117 Uiso 1 1 calc R
H8 H -0.0071 0.7669 0.0636 0.117 Uiso 1 1 calc R
C8 C -0.1203(3) 0.5839(3) -0.0434(5) 0.0726(12) Uani 1 1 d .
H10 H -0.1739 0.5774 0.0113 0.087 Uiso 1 1 calc R
C12 C -0.1254(5) 0.8079(5) -0.0207(10) 0.172(3) Uani 1 1 d .
H4 H -0.0876 0.8557 -0.0619 0.258 Uiso 1 1 calc R
H5 H -0.1666 0.8342 0.0499 0.258 Uiso 1 1 calc R
H6 H -0.1606 0.7789 -0.0967 0.258 Uiso 1 1 calc R
C9 C 0.0062(3) 0.6416(3) -0.1332(4) 0.0618(11) Uani 1 1 d .
H11 H 0.0556 0.6808 -0.1516 0.074 Uiso 1 1 calc R
O7 O 0.35838(14) 0.73274(17) 0.2643(3) 0.0528(6) 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
Zn Zn 0.2839 1.4301 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
H H 0.0000 0.0000 '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
O4 Zn1 O4 112.86(15) . 2_565
O4 Zn1 O7 107.88(10) . .
O4 Zn1 O7 109.47(10) 2_565 .
O4 Zn1 O7 109.47(10) . 2_565
O4 Zn1 O7 107.88(10) 2_565 2_565
O7 Zn1 O7 109.23(14) . 2_565
O6 S1 O5 113.80(16) . .
O6 S1 O4 107.97(14) . .
O5 S1 O4 110.34(15) . .
O6 S1 O7 108.24(15) . 4_464
O5 S1 O7 109.69(14) . 4_464
O4 S1 O7 106.50(16) . 4_464
S1 O4 Zn1 126.45(13) . .
C9 N2 C7 108.4(3) . .
C9 N2 C10 125.8(3) . .
C7 N2 C10 125.8(3) . .
C9 N3 C8 108.7(3) . .
C9 N3 C11 124.2(4) . .
C8 N3 C11 127.1(4) . .
C8 C7 N2 107.3(3) . .
C12 C11 N3 111.6(5) . .
C7 C8 N3 106.7(3) . .
N3 C9 N2 109.0(3) . .
S1 O7 Zn1 127.65(13) 3_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O4 1.950(2) .
Zn1 O4 1.950(2) 2_565
Zn1 O7 1.950(2) .
Zn1 O7 1.950(2) 2_565
S1 O6 1.441(2) .
S1 O5 1.446(2) .
S1 O4 1.482(2) .
S1 O7 1.488(2) 4_464
N2 C9 1.319(4) .
N2 C7 1.362(5) .
N2 C10 1.459(5) .
N3 C9 1.304(5) .
N3 C8 1.374(5) .
N3 C11 1.464(5) .
C7 C8 1.336(6) .
C11 C12 1.426(8) .
O7 S1 1.488(2) 3_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O6 S1 O4 Zn1 146.17(19) . .
O5 S1 O4 Zn1 21.2(2) . .
O7 S1 O4 Zn1 -97.8(2) 4_464 .
O4 Zn1 O4 S1 44.04(16) 2_565 .
O7 Zn1 O4 S1 -77.0(2) . .
O7 Zn1 O4 S1 164.20(18) 2_565 .
C9 N2 C7 C8 1.2(5) . .
C10 N2 C7 C8 -179.8(4) . .
C9 N3 C11 C12 93.4(7) . .
C8 N3 C11 C12 -83.8(7) . .
N2 C7 C8 N3 -1.3(5) . .
C9 N3 C8 C7 0.9(5) . .
C11 N3 C8 C7 178.5(5) . .
C8 N3 C9 N2 -0.2(5) . .
C11 N3 C9 N2 -177.8(4) . .
C7 N2 C9 N3 -0.6(5) . .
C10 N2 C9 N3 -179.6(4) . .
O4 Zn1 O7 S1 -166.15(17) . 3_655
O4 Zn1 O7 S1 70.7(2) 2_565 3_655
O7 Zn1 O7 S1 -47.24(15) 2_565 3_655
