#------------------------------------------------------------------------------
#$Date: 2016-12-18 23:47:55 +0200 (Sun, 18 Dec 2016) $
#$Revision: 189207 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/51/30/1513065.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_1513065
loop_
_publ_author_name
'Storp, Jüergen'
'Stolle, Cornelia'
'Ivanova, Bojidarka'
'Spiteller, Michael'
_publ_section_title
;
 Crystal structures and physical properties of 5-sulfosalicylate and
 violurate metal-organic crystals – experimental vs. theoretical
 study
;
_journal_name_full               'Journal of Coordination Chemistry'
_journal_page_first              2055
_journal_paper_doi               10.1080/00958972.2012.720756
_journal_volume                  65
_journal_year                    2012
_chemical_formula_sum            'C4 H2 K N3 O6'
_chemical_formula_weight         227.19
_chemical_name_common            'potassium violurate dihydrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 105.347(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.296(5)
_cell_length_b                   11.981(4)
_cell_length_c                   6.493(3)
_cell_measurement_temperature    199(2)
_cell_volume                     847.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker GIS'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      199(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_sigmaI/netI    0.1932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5138
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_correction_T_min  0.9330
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0616
_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)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                821
_reflns_number_total             1504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Struct-196A-newsolv.CIF
_cod_data_source_block           bi196a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:
'__diffrn_radiation_source' tag replaced with
'_diffrn_radiation_source'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_cell_volume        847.3(6)
_cod_original_sg_symbol_Hall     '- P 2ybc'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1513065
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, 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
_atom_site_attached_hydrogens
K1 K 0.84590(10) 0.00452(8) 0.11352(18) 0.0324(4) Uani 1 1 d . 0
N3 N 0.4747(3) 0.7116(3) 0.2340(6) 0.0242(10) Uani 1 1 d . 0
H3 H 0.4311 0.6500 0.2052 0.029 Uiso 1 1 calc R 0
O3 O 0.6438(3) 0.6052(2) 0.3638(5) 0.0283(9) Uani 1 1 d . 0
O2 O 0.3041(3) 0.8146(2) 0.1001(5) 0.0342(9) Uani 1 1 d . 0
O1 O 0.8566(3) 0.7238(2) 0.5049(6) 0.0361(10) Uani 1 1 d . 0
N2 N 0.7929(3) 0.8115(3) 0.4512(6) 0.0284(10) Uani 1 1 d . 0
N1 N 0.4826(3) 0.9043(3) 0.2354(6) 0.0256(10) Uani 1 1 d . 0
H1 H 0.4432 0.9683 0.2126 0.031 Uiso 1 1 calc R 0
C4 C 0.6093(4) 0.9089(4) 0.3199(7) 0.0209(11) Uani 1 1 d . 0
C3 C 0.6019(4) 0.7005(4) 0.3275(7) 0.0195(11) Uani 1 1 d . 0
C2 C 0.6699(4) 0.8024(3) 0.3677(7) 0.0199(11) Uani 1 1 d . 0
OW2 O 1.0937(3) 0.8195(2) 0.5995(6) 0.0436(10) Uani 1 1 d . 2
C1 C 0.4142(4) 0.8103(3) 0.1849(7) 0.0218(11) Uani 1 1 d . 0
O4 O 0.6595(3) 1.0018(2) 0.3447(5) 0.0302(9) Uani 1 1 d . 0
OW1 O 0.9059(3) 0.4797(3) 0.2254(6) 0.0442(10) Uani 1 1 d . 2
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'
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
OW1 K1 O3 141.04(10) 2_745 4_565
OW1 K1 OW2 77.36(10) 2_745 3_766
O3 K1 OW2 140.74(11) 4_565 3_766
OW1 K1 OW1 83.28(11) 2_745 4_565
O3 K1 OW1 82.08(11) 4_565 4_565
OW2 K1 OW1 118.72(11) 3_766 4_565
OW1 K1 O1 83.30(9) 2_745 4_565
O3 K1 O1 58.49(8) 4_565 4_565
OW2 K1 O1 151.68(10) 3_766 4_565
OW1 K1 O1 78.68(11) 4_565 4_565
OW1 K1 O2 132.87(10) 2_745 3_665
O3 K1 O2 77.57(9) 4_565 3_665
OW2 K1 O2 76.11(9) 3_766 3_665
OW1 K1 O2 76.44(10) 4_565 3_665
O1 K1 O2 131.79(9) 4_565 3_665
OW1 K1 O4 127.85(12) 2_745 1_545
O3 K1 O4 72.34(10) 4_565 1_545
OW2 K1 O4 75.13(10) 3_766 1_545
OW1 K1 O4 148.86(11) 4_565 1_545
O1 K1 O4 101.73(10) 4_565 1_545
O2 K1 O4 80.88(10) 3_665 1_545
OW1 K1 N2 91.00(10) 2_745 1_545
O3 K1 N2 78.01(9) 4_565 1_545
OW2 K1 N2 98.03(11) 3_766 1_545
OW1 K1 N2 140.20(10) 4_565 1_545
O1 K1 N2 61.54(10) 4_565 1_545
O2 K1 N2 130.74(10) 3_665 1_545
O4 K1 N2 51.05(9) 1_545 1_545
OW1 K1 C4 129.04(12) 2_745 1_545
O3 K1 C4 57.97(10) 4_565 1_545
OW2 K1 C4 93.94(11) 3_766 1_545
OW1 K1 C4 139.95(10) 4_565 1_545
O1 K1 C4 82.31(11) 4_565 1_545
O2 K1 C4 91.09(10) 3_665 1_545
O4 K1 C4 19.75(9) 1_545 1_545
N2 K1 C4 39.92(9) 1_545 1_545
OW1 K1 K1 42.06(9) 2_745 3_755
O3 K1 K1 115.02(9) 4_565 3_755
OW2 K1 K1 100.32(9) 3_766 3_755
OW1 K1 K1 41.21(7) 4_565 3_755
O1 K1 K1 77.89(8) 4_565 3_755
O2 K1 K1 107.05(9) 3_665 3_755
O4 K1 K1 169.89(8) 1_545 3_755
N2 K1 K1 122.00(8) 1_545 3_755
C4 K1 K1 159.11(8) 1_545 3_755
C1 N3 C3 125.0(4) . .
C3 O3 K1 140.2(3) . 4_566
C1 O2 K1 130.5(3) . 3_665
N2 O1 K1 144.0(3) . 4_566
O1 N2 C2 119.3(4) . .
O1 N2 K1 124.4(3) . 1_565
C2 N2 K1 97.8(3) . 1_565
C1 N1 C4 126.1(4) . .
O4 C4 N1 118.3(4) . .
O4 C4 C2 126.3(4) . .
N1 C4 C2 115.4(4) . .
O4 C4 K1 52.0(3) . 1_565
N1 C4 K1 132.5(3) . 1_565
C2 C4 K1 90.3(3) . 1_565
O3 C3 N3 117.7(4) . .
O3 C3 C2 126.5(4) . .
N3 C3 C2 115.8(4) . .
N2 C2 C3 125.9(4) . .
N2 C2 C4 113.1(4) . .
C3 C2 C4 121.0(4) . .
O2 C1 N1 121.4(4) . .
O2 C1 N3 122.0(4) . .
N1 C1 N3 116.5(4) . .
C4 O4 K1 108.3(3) . 1_565
K1 OW1 K1 96.72(11) 2_755 4_566
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 OW1 2.737(4) 2_745
K1 O3 2.758(3) 4_565
K1 OW2 2.776(3) 3_766
K1 OW1 2.783(4) 4_565
K1 O1 2.835(3) 4_565
K1 O2 2.872(3) 3_665
K1 O4 2.892(4) 1_545
K1 N2 3.347(4) 1_545
K1 C4 3.485(5) 1_545
K1 K1 4.126(3) 3_755
N3 C1 1.361(5) .
N3 C3 1.410(5) .
O3 C3 1.235(5) .
O3 K1 2.758(3) 4_566
O2 C1 1.221(5) .
O2 K1 2.872(3) 3_665
O1 N2 1.269(4) .
O1 K1 2.835(3) 4_566
N2 C2 1.356(5) .
N2 K1 3.347(4) 1_565
N1 C1 1.355(5) .
N1 C4 1.392(5) .
C4 O4 1.240(5) .
C4 C2 1.443(6) .
C4 K1 3.485(5) 1_565
C3 C2 1.429(6) .
OW2 K1 2.776(3) 3_766
O4 K1 2.892(4) 1_565
OW1 K1 2.737(4) 2_755
OW1 K1 2.783(4) 4_566
