#------------------------------------------------------------------------------
#$Date: 2016-01-07 04:56:13 +0100 (jue 07 de ene de 2016) $
#$Revision: 173631 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/83/7118377.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_7118377
loop_
_publ_author_name
'Tiwari, Ranjay K.'
'Kumar, Jitendra'
'Behera, J. N.'
_publ_section_title
;
 The first organically templated open-framework metal-sulfites with
 layered and three-dimensional diamondoid structures.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1282
_journal_page_last               1285
_journal_paper_doi               10.1039/c5cc07874a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'O6 S2 Zn, 2(C H6 N3)'
_chemical_formula_sum            'C2 H12 N6 O6 S2 Zn'
_chemical_formula_weight         345.67
_chemical_name_systematic        (Guanidinium)zincsulfite
_chemical_properties_physical    Heat-sensitive
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-15 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.4211(13)
_cell_length_b                   12.1181(8)
_cell_length_c                   14.0692(8)
_cell_measurement_reflns_used    1109
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     2458.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.1040
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9404
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.365
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.868
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1408
_exptl_crystal_recrystallization_method hydrothermal
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.09(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1109
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0380
_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)+(0.0287P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                939
_reflns_number_total             1109
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc07874a2.cif
_cod_data_source_block           complex2
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               7118377
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x+1/4, y+1/4, z+1/4'
'x+1/4, -y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+1/4, -y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+3/4, -y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
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 -0.2500 1.01900(5) 0.02092(19) Uani 1 2 d S
S1 S 0.16309(8) -0.13374(9) 1.18859(9) 0.0231(3) Uani 1 1 d .
O1 O 0.2214(2) -0.1210(3) 1.0965(2) 0.0283(8) Uani 1 1 d .
O2 O 0.2239(3) -0.0956(4) 1.2665(3) 0.0514(11) Uani 1 1 d .
O3 O 0.0917(3) -0.0427(3) 1.1738(3) 0.0467(11) Uani 1 1 d .
N3 N 0.4517(4) 0.1929(4) 1.2073(4) 0.0571(16) Uani 1 1 d .
H3A H 0.4541 0.2423 1.2511 0.069 Uiso 1 1 calc R
H3B H 0.4937 0.1910 1.1639 0.069 Uiso 1 1 calc R
C1 C 0.3837(4) 0.1202(5) 1.2066(4) 0.0395(14) Uani 1 1 d .
N2 N 0.3805(4) 0.0460(4) 1.1377(4) 0.0554(15) Uani 1 1 d .
H2A H 0.3361 -0.0012 1.1359 0.066 Uiso 1 1 calc R
H2B H 0.4230 0.0450 1.0948 0.066 Uiso 1 1 calc R
N1 N 0.3199(4) 0.1227(4) 1.2720(4) 0.0679(18) Uani 1 1 d .
H1A H 0.3220 0.1719 1.3160 0.081 Uiso 1 1 calc R
H1B H 0.2757 0.0751 1.2713 0.081 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0210(4) 0.0242(4) 0.0176(3) 0.000 0.000 0.0008(4)
S1 0.0248(6) 0.0246(6) 0.0199(5) 0.0022(5) 0.0039(5) 0.0011(5)
O1 0.034(2) 0.0243(18) 0.0267(16) -0.0004(14) 0.0159(14) 0.0056(14)
O2 0.048(2) 0.076(3) 0.0306(19) -0.003(2) -0.009(2) -0.001(2)
O3 0.040(2) 0.064(3) 0.036(2) 0.023(2) 0.0166(18) 0.033(2)
N3 0.075(4) 0.053(4) 0.043(3) -0.019(3) 0.019(3) -0.029(3)
C1 0.049(3) 0.040(3) 0.030(3) -0.013(2) 0.009(2) -0.013(3)
N2 0.052(3) 0.060(4) 0.055(3) -0.036(3) 0.023(2) -0.022(3)
N1 0.080(4) 0.069(4) 0.054(3) -0.030(3) 0.037(3) -0.027(3)
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'
O O 0.0106 0.0060 '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'
Zn Zn 0.2839 1.4301 '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
O1 Zn1 O1 112.0(2) . 14_545
O1 Zn1 O3 116.92(17) . 7_544
O1 Zn1 O3 108.31(15) 14_545 7_544
O1 Zn1 O3 108.31(15) . 8_544
O1 Zn1 O3 116.92(17) 14_545 8_544
O3 Zn1 O3 93.4(2) 7_544 8_544
O2 S1 O3 106.0(3) . .
O2 S1 O1 105.5(2) . .
O3 S1 O1 100.38(19) . .
S1 O1 Zn1 120.09(19) . .
S1 O3 Zn1 123.8(2) . 3
N1 C1 N3 120.4(5) . .
N1 C1 N2 120.6(5) . .
N3 C1 N2 119.0(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 1.950(3) .
Zn1 O1 1.950(3) 14_545
Zn1 O3 1.952(3) 7_544
Zn1 O3 1.952(3) 8_544
S1 O2 1.478(4) .
S1 O3 1.523(3) .
S1 O1 1.553(3) .
O3 Zn1 1.952(3) 3
N3 C1 1.319(7) .
C1 N1 1.301(7) .
C1 N2 1.323(6) .
