#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:05:10 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180059 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/05/7050591.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_7050591
loop_
_publ_author_name
'Mezei, Gellert'
'Raptis, Raphael G.'
_publ_section_title
;
 Pyrazole-4-sulfonate networks of alkali and alkaline-earth metals.
 Effect of cation size, charge, H-bonding and aromatic interactions on
 the three-dimensional supramolecular architecture
;
_journal_issue                   9
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1399
_journal_paper_doi               10.1039/b303096b
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C3 H5 K N2 O4 S'
_chemical_formula_weight         204.25
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   8.1743(12)
_cell_length_b                   8.9723(13)
_cell_length_c                   19.912(3)
_cell_measurement_temperature    298(2)
_cell_volume                     1460.4(4)
_computing_cell_refinement       'BRUKER SMART-NT V5.0'
_computing_data_collection       'BRUKER SMART-NT V5.0'
_computing_data_reduction        'BRUKER SAINT-NT V5/6.0'
_computing_molecular_graphics    'BRUKER SHELXTL-NT V5.1'
_computing_publication_material  'BRUKER SHELXTL-NT V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0855
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5775
_diffrn_reflns_theta_full        23.27
_diffrn_reflns_theta_max         23.27
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.302
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     108
_refine_ls_number_reflns         1047
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0568
_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)+(0.1150P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1517
_reflns_number_gt                864
_reflns_number_total             1047
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303096b.txt
_cod_data_source_block           K(4-SO3-pzH).H2O
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7050591
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.0710(5) 0.3290(5) 0.4829(2) 0.0299(10) Uani 1 1 d . . .
H1 H -0.0203 0.2679 0.4785 0.036 Uiso 1 1 calc R . .
C2 C 0.1581(4) 0.3945(4) 0.4317(2) 0.0189(9) Uani 1 1 d . . .
C3 C 0.2815(5) 0.4764(5) 0.4640(2) 0.0286(10) Uani 1 1 d . . .
H3 H 0.3588 0.5344 0.4418 0.034 Uiso 1 1 calc R . .
H1O H 0.128(5) 0.422(4) 0.1163(17) 0.039(14) Uiso 1 1 d D . .
H2O H 0.015(4) 0.393(8) 0.159(3) 0.10(3) Uiso 1 1 d D . .
K1 K 0.25773(10) 0.13997(10) 0.22742(5) 0.0251(4) Uani 1 1 d . . .
N1 N 0.2733(4) 0.4604(5) 0.53049(17) 0.0369(10) Uani 1 1 d . . .
N2 N 0.1422(4) 0.3699(4) 0.53981(19) 0.0343(10) Uani 1 1 d . . .
H2 H 0.1087 0.3418 0.5788 0.041 Uiso 1 1 calc R . .
O1 O 0.2737(3) 0.3919(3) 0.31255(15) 0.0278(8) Uani 1 1 d . . .
O2 O 0.0292(3) 0.2501(3) 0.33470(14) 0.0365(8) Uani 1 1 d . . .
O3 O 0.0186(3) 0.5196(3) 0.33028(13) 0.0338(8) Uani 1 1 d . . .
O4 O 0.1093(4) 0.3697(4) 0.14922(18) 0.0400(9) Uani 1 1 d D . .
S1 S 0.11498(11) 0.38837(11) 0.34587(5) 0.0203(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
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'
K K 0.2009 0.2494 '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'
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
_geom_angle_publ_flag
N2 C1 C2 106.7(4) . . ?
C1 C2 C3 104.9(4) . . ?
C1 C2 S1 127.4(3) . . ?
C3 C2 S1 127.6(3) . . ?
N1 C3 C2 111.2(4) . . ?
O2 K1 O3 128.35(10) 6_656 3_545 ?
O2 K1 O1 129.45(9) 6_656 8_655 ?
O3 K1 O1 82.30(9) 3_545 8_655 ?
O2 K1 O1 86.82(9) 6_656 . ?
O3 K1 O1 126.95(9) 3_545 . ?
O1 K1 O1 106.01(10) 8_655 . ?
O2 K1 O4 80.60(10) 6_656 . ?
O3 K1 O4 72.96(10) 3_545 . ?
O1 K1 O4 149.59(9) 8_655 . ?
O1 K1 O4 76.68(10) . . ?
O2 K1 O3 86.75(8) 6_656 8_655 ?
O3 K1 O3 130.86(11) 3_545 8_655 ?
O1 K1 O3 49.29(8) 8_655 8_655 ?
O1 K1 O3 81.24(8) . 8_655 ?
O4 K1 O3 155.04(10) . 8_655 ?
O2 K1 O2 135.19(11) 6_656 . ?
O3 K1 O2 85.16(8) 3_545 . ?
O1 K1 O2 76.98(9) 8_655 . ?
O1 K1 O2 48.69(8) . . ?
O4 K1 O2 83.46(9) . . ?
O3 K1 O2 90.69(9) 8_655 . ?
O2 K1 O4 76.63(9) 6_656 8_655 ?
O3 K1 O4 76.69(9) 3_545 8_655 ?
O1 K1 O4 73.35(9) 8_655 8_655 ?
O1 K1 O4 156.33(9) . 8_655 ?
O4 K1 O4 116.28(13) . 8_655 ?
O3 K1 O4 81.03(9) 8_655 8_655 ?
O2 K1 O4 146.89(9) . 8_655 ?
O2 K1 S1 107.69(7) 6_656 8_655 ?
O3 K1 S1 106.13(7) 3_545 8_655 ?
O1 K1 S1 24.58(6) 8_655 8_655 ?
O1 K1 S1 95.73(6) . 8_655 ?
O4 K1 S1 168.65(8) . 8_655 ?
O3 K1 S1 24.88(6) 8_655 8_655 ?
O2 K1 S1 85.19(6) . 8_655 ?
O4 K1 S1 73.87(7) 8_655 8_655 ?
O2 K1 S1 110.58(7) 6_656 . ?
O3 K1 S1 105.14(7) 3_545 . ?
O1 K1 S1 93.92(7) 8_655 . ?
O1 K1 S1 24.39(6) . . ?
O4 K1 S1 76.27(8) . . ?
O3 K1 S1 88.36(6) 8_655 . ?
O2 K1 S1 24.61(6) . . ?
O4 K1 S1 166.91(7) 8_655 . ?
S1 K1 S1 93.31(3) 8_655 . ?
O2 K1 K1 45.77(6) 6_656 6_656 ?
O3 K1 K1 152.93(7) 3_545 6_656 ?
O1 K1 K1 87.69(6) 8_655 6_656 ?
O1 K1 K1 79.98(6) . 6_656 ?
O4 K1 K1 122.17(7) . 6_656 ?
O3 K1 K1 41.03(5) 8_655 6_656 ?
O2 K1 K1 117.02(6) . 6_656 ?
O4 K1 K1 76.35(7) 8_655 6_656 ?
S1 K1 K1 63.61(3) 8_655 6_656 ?
S1 K1 K1 100.57(3) . 6_656 ?
O2 K1 K1 153.20(7) 6_656 6_556 ?
O3 K1 K1 44.66(6) 3_545 6_556 ?
O1 K1 K1 77.35(6) 8_655 6_556 ?
O1 K1 K1 85.20(6) . 6_556 ?
O4 K1 K1 72.67(7) . 6_556 ?
O3 K1 K1 117.13(6) 8_655 6_556 ?
O2 K1 K1 40.55(5) . 6_556 ?
O4 K1 K1 116.95(7) 8_655 6_556 ?
S1 K1 K1 98.55(3) 8_655 6_556 ?
S1 K1 K1 61.48(3) . 6_556 ?
K1 K1 K1 155.18(5) 6_656 6_556 ?
C3 N1 N2 103.9(3) . . ?
C1 N2 N1 113.3(4) . . ?
S1 O1 K1 102.14(13) . 8_665 ?
S1 O1 K1 102.37(15) . . ?
K1 O1 K1 105.50(10) 8_665 . ?
S1 O2 K1 141.04(18) . 6_556 ?
S1 O2 K1 95.18(14) . . ?
K1 O2 K1 93.68(8) 6_556 . ?
S1 O3 K1 148.52(18) . 3 ?
S1 O3 K1 96.28(13) . 8_665 ?
K1 O3 K1 94.31(8) 3 8_665 ?
K1 O4 K1 98.21(11) . 8_665 ?
O2 S1 O3 113.67(19) . . ?
O2 S1 O1 112.41(17) . . ?
O3 S1 O1 111.62(17) . . ?
O2 S1 C2 106.04(17) . . ?
O3 S1 C2 107.08(17) . . ?
O1 S1 C2 105.37(18) . . ?
O2 S1 K1 127.45(12) . 8_665 ?
O3 S1 K1 58.85(12) . 8_665 ?
O1 S1 K1 53.28(11) . 8_665 ?
C2 S1 K1 126.28(13) . 8_665 ?
O2 S1 K1 60.20(12) . . ?
O3 S1 K1 124.20(12) . . ?
O1 S1 K1 53.24(12) . . ?
C2 S1 K1 128.42(13) . . ?
K1 S1 K1 81.50(3) 8_665 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N2 1.326(6) . ?
C1 C2 1.375(6) . ?
C2 C3 1.403(5) . ?
C2 S1 1.746(4) . ?
C3 N1 1.334(5) . ?
K1 O2 2.726(3) 6_656 ?
K1 O3 2.755(3) 3_545 ?
K1 O1 2.810(3) 8_655 ?
K1 O1 2.828(3) . ?
K1 O4 2.854(4) . ?
K1 O3 2.950(3) 8_655 ?
K1 O2 3.005(3) . ?
K1 O4 3.080(4) 8_655 ?
K1 S1 3.4267(13) 8_655 ?
K1 S1 3.4484(13) . ?
K1 K1 4.1849(7) 6_656 ?
K1 K1 4.1849(7) 6_556 ?
N1 N2 1.358(5) . ?
O1 S1 1.458(3) . ?
O1 K1 2.810(3) 8_665 ?
O2 S1 1.442(3) . ?
O2 K1 2.726(3) 6_556 ?
O3 S1 1.450(3) . ?
O3 K1 2.755(3) 3 ?
O3 K1 2.950(3) 8_665 ?
O4 K1 3.080(4) 8_665 ?
S1 K1 3.4267(13) 8_665 ?
