#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:16:36 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180420 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/89/7208976.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_7208976
loop_
_publ_author_name
'Lucas, Jacqueline S.'
'Uebler, Jacob W.'
'LaDuca, Robert L.'
_publ_section_title
;
 Metal dependent dimensionality in sulfate coordination polymers
 containing 3-pyridylisonicotinamide
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              860
_journal_paper_doi               10.1039/c2ce26333e
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C11 H13 Cu N3 O7 S'
_chemical_formula_weight         394.84
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2012-06-12 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 122.425(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.075(7)
_cell_length_b                   9.496(3)
_cell_length_c                   14.226(4)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.36
_cell_volume                     2745.2(14)
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0612
_diffrn_reflns_av_sigmaI/netI    0.0486
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10721
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.40
_diffrn_reflns_theta_min         2.00
_exptl_absorpt_coefficient_mu    1.787
_exptl_absorpt_correction_T_max  0.7642
_exptl_absorpt_correction_T_min  0.6498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.088
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         2534
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0412
_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)+(0.0749P)²+3.1309P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                2192
_reflns_number_total             2534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce26333e.txt
_cod_data_source_block           c2c
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7208976
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Cu1 Cu 0.247651(17) 0.04550(4) 0.35342(3) 0.01560(17) Uani 1 1 d .
S2 S 0.32022(3) -0.17397(8) 0.24928(6) 0.0138(2) Uani 1 1 d .
O1 O 0.26251(12) -0.0291(2) 0.4953(2) 0.0213(5) Uani 1 1 d D
H1A H 0.2313(14) -0.059(4) 0.499(3) 0.026 Uiso 1 1 d D
H1B H 0.2782(17) 0.039(3) 0.541(3) 0.026 Uiso 1 1 d D
O1W O 0.33503(12) -0.3817(3) 0.4830(2) 0.0261(6) Uani 1 1 d D
H1WA H 0.3168(18) -0.362(4) 0.4153(16) 0.031 Uiso 1 1 d D
H1WB H 0.3639(15) -0.324(3) 0.524(3) 0.031 Uiso 1 1 d D
O2 O 0.44620(11) -0.2130(2) 0.6083(2) 0.0236(5) Uani 1 1 d .
O3 O 0.28306(11) -0.0552(2) 0.25482(19) 0.0191(5) Uani 1 1 d .
O4 O 0.38998(11) -0.1639(2) 0.3362(2) 0.0221(5) Uani 1 1 d .
O5 O 0.31056(12) -0.1812(2) 0.13887(19) 0.0247(6) Uani 1 1 d .
O6 O 0.29359(10) -0.3083(2) 0.26642(18) 0.0169(5) Uani 1 1 d .
N1 N 0.33694(12) 0.1334(3) 0.4495(2) 0.0157(6) Uani 1 1 d .
N2 N 0.50353(13) -0.0166(3) 0.6218(2) 0.0183(6) Uani 1 1 d D
H2N H 0.5427(12) 0.018(4) 0.641(3) 0.022 Uiso 1 1 d D
N3 N 0.66670(13) -0.4239(3) 0.7736(2) 0.0174(6) Uani 1 1 d .
C1 C 0.38634(15) 0.0403(3) 0.4994(3) 0.0168(7) Uani 1 1 d .
H1 H 0.3769 -0.0569 0.4825 0.020 Uiso 1 1 calc R
C2 C 0.45055(15) 0.0806(3) 0.5745(3) 0.0172(7) Uani 1 1 d .
C3 C 0.46398(15) 0.2214(4) 0.5999(3) 0.0219(7) Uani 1 1 d .
H3 H 0.5077 0.2523 0.6513 0.026 Uiso 1 1 calc R
C4 C 0.41292(16) 0.3163(3) 0.5495(3) 0.0246(8) Uani 1 1 d .
H4 H 0.4211 0.4137 0.5668 0.030 Uiso 1 1 calc R
C5 C 0.34957(15) 0.2702(3) 0.4735(3) 0.0190(7) Uani 1 1 d .
H5 H 0.3147 0.3366 0.4381 0.023 Uiso 1 1 calc R
C6 C 0.60572(18) -0.4733(4) 0.7052(3) 0.0291(8) Uani 1 1 d .
H6 H 0.5998 -0.5711 0.6883 0.035 Uiso 1 1 calc R
C7 C 0.55132(16) -0.3873(4) 0.6587(3) 0.0305(9) Uani 1 1 d .
H7 H 0.5086 -0.4259 0.6114 0.037 Uiso 1 1 calc R
C8 C 0.55915(15) -0.2435(3) 0.6811(3) 0.0172(6) Uani 1 1 d .
C9 C 0.62217(15) -0.1934(3) 0.7491(3) 0.0198(7) Uani 1 1 d .
H9 H 0.6297 -0.0956 0.7649 0.024 Uiso 1 1 calc R
C10 C 0.67421(15) -0.2860(3) 0.7941(3) 0.0196(7) Uani 1 1 d .
H10 H 0.7174 -0.2500 0.8419 0.024 Uiso 1 1 calc R
C11 C 0.49799(15) -0.1562(3) 0.6332(3) 0.0175(7) 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'
S S 0.1246 0.1234 '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'
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 Cu1 O6 148.40(10) . 4
O1 Cu1 N1 84.98(10) . .
O6 Cu1 N1 98.78(10) 4 .
O1 Cu1 N3 87.75(10) . 8_445
O6 Cu1 N3 91.68(10) 4 8_445
N1 Cu1 N3 169.08(11) . 8_445
O1 Cu1 O3 124.80(9) . .
O6 Cu1 O3 86.76(9) 4 .
N1 Cu1 O3 88.59(10) . .
N3 Cu1 O3 88.87(10) 8_445 .
O4 S2 O5 111.20(14) . .
O4 S2 O3 111.19(14) . .
O5 S2 O3 110.09(13) . .
O4 S2 O6 108.33(13) . .
O5 S2 O6 107.36(13) . .
O3 S2 O6 108.54(12) . .
Cu1 O1 H1A 121(3) . .
Cu1 O1 H1B 105(3) . .
H1A O1 H1B 105(3) . .
H1WA O1W H1WB 112(3) . .
S2 O3 Cu1 145.04(14) . .
S2 O6 Cu1 120.65(13) . 4_545
C5 N1 C1 119.4(3) . .
C5 N1 Cu1 126.3(2) . .
C1 N1 Cu1 114.1(2) . .
C11 N2 C2 125.0(3) . .
C11 N2 H2N 119(3) . .
C2 N2 H2N 116(3) . .
C10 N3 C6 118.1(3) . .
C10 N3 Cu1 117.6(2) . 8_546
C6 N3 Cu1 124.2(2) . 8_546
N1 C1 C2 122.3(3) . .
N1 C1 H1 118.8 . .
C2 C1 H1 118.8 . .
C3 C2 C1 118.7(3) . .
C3 C2 N2 118.8(3) . .
C1 C2 N2 122.4(3) . .
C4 C3 C2 118.7(3) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
C3 C4 C5 120.1(3) . .
C3 C4 H4 119.9 . .
C5 C4 H4 119.9 . .
N1 C5 C4 120.7(3) . .
N1 C5 H5 119.6 . .
C4 C5 H5 119.6 . .
N3 C6 C7 122.2(3) . .
N3 C6 H6 118.9 . .
C7 C6 H6 118.9 . .
C6 C7 C8 119.7(3) . .
C6 C7 H7 120.2 . .
C8 C7 H7 120.2 . .
C9 C8 C7 117.6(3) . .
C9 C8 C11 125.0(3) . .
C7 C8 C11 117.3(3) . .
C8 C9 C10 119.5(3) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
N3 C10 C9 122.9(3) . .
N3 C10 H10 118.5 . .
C9 C10 H10 118.5 . .
O2 C11 N2 123.3(3) . .
O2 C11 C8 119.2(3) . .
N2 C11 C8 117.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.982(2) .
Cu1 O6 2.001(2) 4
Cu1 N1 2.009(3) .
Cu1 N3 2.012(3) 8_445
Cu1 O3 2.212(2) .
S2 O4 1.460(2) .
S2 O5 1.461(2) .
S2 O3 1.468(2) .
S2 O6 1.505(2) .
O1 H1A 0.829(18) .
O1 H1B 0.851(18) .
O1W H1WA 0.839(18) .
O1W H1WB 0.827(18) .
O2 C11 1.224(4) .
O6 Cu1 2.001(2) 4_545
N1 C5 1.337(4) .
N1 C1 1.340(4) .
N2 C11 1.351(4) .
N2 C2 1.418(4) .
N2 H2N 0.892(18) .
N3 C10 1.333(4) .
N3 C6 1.338(4) .
N3 Cu1 2.012(3) 8_546
C1 C2 1.381(4) .
C1 H1 0.9500 .
C2 C3 1.378(5) .
C3 C4 1.376(5) .
C3 H3 0.9500 .
C4 C5 1.385(4) .
C4 H4 0.9500 .
C5 H5 0.9500 .
C6 C7 1.375(5) .
C6 H6 0.9500 .
C7 C8 1.393(5) .
C7 H7 0.9500 .
C8 C9 1.375(4) .
C8 C11 1.498(4) .
C9 C10 1.376(4) .
C9 H9 0.9500 .
C10 H10 0.9500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1A O1W 0.829(18) 1.838(19) 2.666(3) 175(4) 7_546
O1 H1B O5 0.851(18) 1.789(19) 2.639(3) 178(4) 6_556
O1W H1WA O6 0.839(18) 1.95(2) 2.771(3) 168(4) .
O1W H1WB O2 0.827(18) 1.98(2) 2.791(3) 165(4) .
N2 H2N O4 0.892(18) 2.02(2) 2.868(4) 158(3) 5_656
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
O4 S2 O3 Cu1 -67.7(3) . .
O5 S2 O3 Cu1 168.6(2) . .
O6 S2 O3 Cu1 51.3(3) . .
O1 Cu1 O3 S2 -1.4(3) . .
O6 Cu1 O3 S2 -179.6(2) 4 .
N1 Cu1 O3 S2 81.5(3) . .
N3 Cu1 O3 S2 -87.9(3) 8_445 .
O4 S2 O6 Cu1 -121.50(15) . 4_545
O5 S2 O6 Cu1 -1.32(18) . 4_545
O3 S2 O6 Cu1 117.65(15) . 4_545
O1 Cu1 N1 C5 -107.9(3) . .
O6 Cu1 N1 C5 40.5(3) 4 .
N3 Cu1 N1 C5 -156.4(5) 8_445 .
O3 Cu1 N1 C5 127.0(3) . .
O1 Cu1 N1 C1 66.4(2) . .
O6 Cu1 N1 C1 -145.2(2) 4 .
N3 Cu1 N1 C1 17.9(7) 8_445 .
O3 Cu1 N1 C1 -58.7(2) . .
C5 N1 C1 C2 -0.7(5) . .
Cu1 N1 C1 C2 -175.4(2) . .
N1 C1 C2 C3 0.8(5) . .
N1 C1 C2 N2 -175.7(3) . .
C11 N2 C2 C3 158.8(3) . .
C11 N2 C2 C1 -24.7(5) . .
C1 C2 C3 C4 0.0(5) . .
N2 C2 C3 C4 176.7(3) . .
C2 C3 C4 C5 -0.9(5) . .
C1 N1 C5 C4 -0.3(5) . .
Cu1 N1 C5 C4 173.8(2) . .
C3 C4 C5 N1 1.1(5) . .
C10 N3 C6 C7 -1.7(5) . .
Cu1 N3 C6 C7 175.3(3) 8_546 .
N3 C6 C7 C8 1.1(6) . .
C6 C7 C8 C9 0.7(5) . .
C6 C7 C8 C11 -176.7(3) . .
C7 C8 C9 C10 -1.6(5) . .
C11 C8 C9 C10 175.5(3) . .
C6 N3 C10 C9 0.7(5) . .
Cu1 N3 C10 C9 -176.5(3) 8_546 .
C8 C9 C10 N3 1.0(5) . .
C2 N2 C11 O2 -3.7(5) . .
C2 N2 C11 C8 177.6(3) . .
C9 C8 C11 O2 -154.4(3) . .
C7 C8 C11 O2 22.7(5) . .
C9 C8 C11 N2 24.4(5) . .
C7 C8 C11 N2 -158.5(3) . .
