#------------------------------------------------------------------------------
#$Date: 2015-10-10 05:18:21 +0300 (Sat, 10 Oct 2015) $
#$Revision: 164415 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/11/2241196.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241196
loop_
_publ_author_name
'Lukianova, Tamara J.'
'Kinzhybalo, Vasyl'
'Pietraszko, Adam'
_publ_section_title
;
 Crystal structure of new organically templated copper sulfate with
 2-aminopyridinium
;
_journal_coeditor_code           HP2072
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m191
_journal_page_last               m192
_journal_paper_doi               10.1107/S2056989015018629
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C5 H7 N2)2 [Cu (H2 O)6] (S O4)2 , 4H2 O'
_chemical_formula_moiety         'Cu H12 O6, 2(O4 S), 2(C5 H7 N2), 4(H2 O)'
_chemical_formula_sum            'C10 H34 Cu N4 O18 S2'
_chemical_formula_weight         626.07
_chemical_name_systematic
;
Bis(2-aminopyridinium) hexaaquacopper(II) bis(sulfate) tetrahydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                91.83(3)
_cell_angle_beta                 104.59(3)
_cell_angle_gamma                114.57(3)
_cell_formula_units_Z            1
_cell_length_a                   7.115(3)
_cell_length_b                   8.211(3)
_cell_length_c                   12.561(4)
_cell_measurement_reflns_used    2602
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.3710
_cell_measurement_theta_min      3.2930
_cell_volume                     638.0(5)
_computing_cell_refinement
;
CrysAlisPro (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
CrysAlisPro  (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
CrysAlisPro  (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1997)
;
_computing_publication_material
;
Olex2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL2014/7 (Sheldrick, 2008)
;
_computing_structure_solution
;
?
SHELXS2014/7 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295.15
_diffrn_detector_area_resol_mean 8.2214
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction Xcalibur, Sapphire2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7926
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.402
_diffrn_reflns_theta_min         3.008
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku Oxford Diffraction, 2015)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_description       block
_exptl_crystal_F_000             327
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.408
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0324P)²+0.2243P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0938
_reflns_number_gt                2268
_reflns_number_total             3173
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hp2072sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        638.0(4)
_cod_database_code               2241196
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.699
_shelx_estimated_absorpt_t_max   0.870
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Cu Cu1 0.5000 0.5000 0.5000 0.03035(15) Uani d 1
O O11W 0.1945(3) 0.4686(3) 0.35088(16) 0.0476(5) Uani d 1
H H11A 0.1489 0.5468 0.3566 0.071 Uiso d 1
H H11B 0.0825 0.3704 0.3272 0.071 Uiso d 1
O O12W 0.3772(3) 0.2434(2) 0.50851(15) 0.0482(6) Uani d 1
H H12A 0.3051 0.1679 0.4500 0.072 Uiso d 1
H H12B 0.3718 0.1983 0.5673 0.072 Uiso d 1
O O13W 0.3680(3) 0.5392(2) 0.61353(14) 0.0359(4) Uani d 1
H H13A 0.3521 0.6347 0.6187 0.054 Uiso d 1
H H13B 0.2510 0.4506 0.6110 0.054 Uiso d 1
S S1 0.34958(11) -0.04901(9) 0.72795(5) 0.03015(17) Uani d 1
O O11 0.5437(3) -0.0526(3) 0.80214(15) 0.0434(5) Uani d 1
O O12 0.1755(3) -0.1167(3) 0.78078(18) 0.0541(6) Uani d 1
O O13 0.3945(4) 0.1366(3) 0.70846(16) 0.0493(6) Uani d 1
O O14 0.2833(4) -0.1658(3) 0.62203(16) 0.0566(6) Uani d 1
N N1 0.6656(4) 0.4231(3) 0.89059(17) 0.0385(6) Uani d 1
H H1 0.6136 0.3421 0.8326 0.046 Uiso calc 1
N N2 0.6983(4) 0.2085(3) 0.99866(19) 0.0462(6) Uani d 1
H H2A 0.6458 0.1297 0.9395 0.055 Uiso calc 1
H H2B 0.7349 0.1784 1.0629 0.055 Uiso calc 1
C C2 0.7227(4) 0.3756(4) 0.9910(2) 0.0364(6) Uani d 1
C C3 0.8066(5) 0.5115(4) 1.0846(2) 0.0484(8) Uani d 1
H H3 0.8482 0.4852 1.1557 0.058 Uiso calc 1
C C4 0.8263(5) 0.6786(4) 1.0711(3) 0.0527(8) Uani d 1
H H4 0.8812 0.7670 1.1334 0.063 Uiso calc 1
C C5 0.7659(5) 0.7227(4) 0.9654(3) 0.0510(8) Uani d 1
H H5 0.7806 0.8391 0.9566 0.061 Uiso calc 1
C C6 0.6855(5) 0.5915(4) 0.8760(3) 0.0477(8) Uani d 1
H H6 0.6441 0.6171 0.8046 0.057 Uiso calc 1
O O14W -0.0364(3) 0.2860(3) 0.59552(16) 0.0432(5) Uani d 1
H H14A -0.0658 0.1958 0.6291 0.065 Uiso d 1
H H14B -0.1086 0.2458 0.5285 0.065 Uiso d 1
O O15W 0.1567(3) 0.0248(2) 0.30825(15) 0.0381(5) Uani d 1
H H15A 0.2371 0.0360 0.2675 0.057 Uiso d 1
H H15B 0.0585 0.0513 0.2734 0.057 Uiso d 1
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'
Cu Cu 0.3201 1.2651 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O11W Cu1 O11W 2_666 . 180.0
O12W Cu1 O11W . . 92.90(9)
O12W Cu1 O11W 2_666 2_666 92.90(9)
O12W Cu1 O11W 2_666 . 87.10(9)
O12W Cu1 O11W . 2_666 87.10(9)
O12W Cu1 O12W 2_666 . 180.0
O12W Cu1 O13W . . 89.66(8)
O12W Cu1 O13W 2_666 2_666 89.66(9)
O12W Cu1 O13W 2_666 . 90.34(8)
O12W Cu1 O13W . 2_666 90.34(8)
O13W Cu1 O11W 2_666 . 88.14(8)
O13W Cu1 O11W . 2_666 88.14(8)
O13W Cu1 O11W 2_666 2_666 91.86(8)
O13W Cu1 O11W . . 91.86(8)
O13W Cu1 O13W . 2_666 180.00(11)
Cu1 O11W H11A . . 115.8
Cu1 O11W H11B . . 122.9
H11A O11W H11B . . 104.7
Cu1 O12W H12A . . 119.8
Cu1 O12W H12B . . 125.3
H12A O12W H12B . . 114.2
Cu1 O13W H13A . . 118.5
Cu1 O13W H13B . . 113.2
H13A O13W H13B . . 108.7
O12 S1 O11 . . 108.78(12)
O13 S1 O11 . . 110.06(13)
O13 S1 O12 . . 109.43(13)
O14 S1 O11 . . 109.47(12)
O14 S1 O12 . . 109.29(15)
O14 S1 O13 . . 109.78(13)
C2 N1 H1 . . 118.2
C2 N1 C6 . . 123.6(2)
C6 N1 H1 . . 118.2
H2A N2 H2B . . 120.0
C2 N2 H2A . . 120.0
C2 N2 H2B . . 120.0
N1 C2 C3 . . 116.8(3)
N2 C2 N1 . . 120.1(2)
N2 C2 C3 . . 123.1(3)
C2 C3 H3 . . 119.9
C4 C3 C2 . . 120.1(3)
C4 C3 H3 . . 119.9
C3 C4 H4 . . 119.3
C3 C4 C5 . . 121.3(3)
C5 C4 H4 . . 119.3
C4 C5 H5 . . 120.9
C6 C5 C4 . . 118.2(3)
C6 C5 H5 . . 120.9
N1 C6 C5 . . 119.9(3)
N1 C6 H6 . . 120.0
C5 C6 H6 . . 120.0
H14A O14W H14B . . 106.1
H15A O15W H15B . . 106.7
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cu1 O11W . 2.398(2)
Cu1 O11W 2_666 2.398(2)
Cu1 O12W 2_666 1.935(2)
Cu1 O12W . 1.935(2)
Cu1 O13W . 1.9790(18)
Cu1 O13W 2_666 1.9790(18)
O11W H11A . 0.8397
O11W H11B . 0.8396
O12W H12A . 0.8396
O12W H12B . 0.8394
O13W H13A . 0.8398
O13W H13B . 0.8398
S1 O11 . 1.471(2)
S1 O12 . 1.466(2)
S1 O13 . 1.464(2)
S1 O14 . 1.462(2)
N1 H1 . 0.8600
N1 C2 . 1.347(3)
N1 C6 . 1.353(4)
N2 H2A . 0.8600
N2 H2B . 0.8600
N2 C2 . 1.319(4)
C2 C3 . 1.412(4)
C3 H3 . 0.9300
C3 C4 . 1.341(4)
C4 H4 . 0.9300
C4 C5 . 1.397(4)
C5 H5 . 0.9300
C5 C6 . 1.355(4)
C6 H6 . 0.9300
O14W H14A . 0.8397
O14W H14B . 0.8397
O15W H15A . 0.8399
O15W H15B . 0.8401
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O11W H11A O14W 2_566 0.84 2.00 2.821(3) 166.6
O11W H11B O12 2_556 0.84 2.22 3.032(4) 162.3
O12W H12A O15W . 0.84 1.88 2.719(3) 172.3
O12W H12B O13 . 0.84 1.85 2.677(3) 170.5
O13W H13A O14 1_565 0.84 1.90 2.733(3) 173.6
O13W H13B O14W . 0.84 1.88 2.706(3) 167.9
N1 H1 O13 . 0.86 2.03 2.855(3) 159.9
N2 H2A O11 . 0.86 2.01 2.869(3) 176.1
N2 H2B O12 2_657 0.86 2.05 2.914(3) 177.6
O14W H14A O15W 2_556 0.84 1.92 2.758(3) 174.0
O14W H14B O14 2_556 0.84 1.90 2.738(3) 175.6
O15W H15A O11 2_656 0.84 1.93 2.761(3) 169.0
O15W H15B O12 2_556 0.84 1.93 2.760(3) 169.6
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
N1 C2 C3 C4 0.0(4)
N2 C2 C3 C4 -179.7(3)
C2 N1 C6 C5 -0.3(5)
C2 C3 C4 C5 -0.2(5)
C3 C4 C5 C6 0.3(5)
C4 C5 C6 N1 0.0(5)
C6 N1 C2 N2 179.9(3)
C6 N1 C2 C3 0.3(4)

_cod_database_fobs_code 2241196
