#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/46/7054641.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_7054641
loop_
_publ_author_name
'Kammoun, Omar'
'Rekik, Walid'
'Naïli, Houcine'
'Bataille, Thierry'
_publ_section_title
;
 Inorganic layered structures in hybrid double sulfates: related phases
 and thermal reactivity
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              2682
_journal_paper_doi               10.1039/C4NJ02195A
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         '2(C7 H7 N2), Ni H12 O6, 2(O4 S), 4(H2 O)'
_chemical_formula_sum            'C14 H34 N4 Ni O18 S2'
_chemical_formula_weight         669.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc13pwsg
_audit_creation_method           SHELXL-97
_audit_update_record
;
2014-11-13 deposited with the CCDC.
2015-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                84.337(2)
_cell_angle_beta                 79.491(2)
_cell_angle_gamma                85.886(2)
_cell_formula_units_Z            1
_cell_length_a                   6.6415(3)
_cell_length_b                   8.2264(4)
_cell_length_c                   12.2601(6)
_cell_measurement_reflns_used    3439
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.33
_cell_measurement_theta_min      2.49
_cell_volume                     654.40(5)
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0502
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10712
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(c.f. r.h. blessing, acta cryst. (1995), a51, 33-38) 
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             350
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2988
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0359
_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)+(0.0630P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                2523
_reflns_number_total             2988
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj02195a2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7054638--7054641.cif.'
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054641
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Ni1 Ni 0.5000 0.5000 1.0000 0.00842(15) Uani 1 2 d S
S1 S 0.10579(8) 0.85964(7) 0.77660(5) 0.00957(17) Uani 1 1 d .
O1 O -0.0455(2) 0.9496(2) 0.85733(14) 0.0153(4) Uani 1 1 d .
O2 O 0.0817(3) 0.6819(2) 0.80337(15) 0.0164(4) Uani 1 1 d .
OW1 O 0.5835(3) 0.1091(2) 0.85273(15) 0.0153(4) Uani 1 1 d D
O4 O 0.3139(2) 0.8981(2) 0.78784(14) 0.0145(4) Uani 1 1 d .
OW4 O 0.5026(3) 0.2562(2) 1.04466(15) 0.0139(4) Uani 1 1 d D
O3 O 0.0679(3) 0.9093(2) 0.66346(14) 0.0164(4) Uani 1 1 d .
OW5 O 0.3617(2) 0.4570(2) 0.86822(14) 0.0126(4) Uani 1 1 d D
OW2 O 0.0738(3) 0.2246(2) 0.93273(15) 0.0151(4) Uani 1 1 d D
C5 C 0.2965(4) 0.2633(3) 0.5676(2) 0.0200(6) Uani 1 1 d .
H5 H 0.2996 0.1804 0.6248 0.024 Uiso 1 1 calc R
OW3 O 0.2192(2) 0.5313(2) 1.10498(14) 0.0133(4) Uani 1 1 d D
N2 N 0.2764(3) 0.6468(3) 0.32882(17) 0.0155(5) Uani 1 1 d .
HN2 H 0.3059 0.6585 0.2573 0.019 Uiso 1 1 calc R
C1 C 0.2077(4) 0.7650(3) 0.3940(2) 0.0164(6) Uani 1 1 d .
H1 H 0.1830 0.8739 0.3692 0.020 Uiso 1 1 calc R
N1 N 0.1795(3) 0.7057(2) 0.49932(17) 0.0140(5) Uani 1 1 d .
HN1 H 0.1355 0.7611 0.5556 0.017 Uiso 1 1 calc R
C3 C 0.3562(4) 0.3422(3) 0.3686(2) 0.0193(6) Uani 1 1 d .
H3 H 0.3965 0.3164 0.2954 0.023 Uiso 1 1 calc R
C2 C 0.2933(3) 0.5006(3) 0.3945(2) 0.0124(5) Uani 1 1 d .
C7 C 0.2326(3) 0.5392(3) 0.5043(2) 0.0120(5) Uani 1 1 d .
C6 C 0.2336(4) 0.4204(3) 0.5939(2) 0.0174(6) Uani 1 1 d .
H6 H 0.1941 0.4458 0.6672 0.021 Uiso 1 1 calc R
C4 C 0.3558(4) 0.2258(3) 0.4568(2) 0.0215(6) Uani 1 1 d .
H4 H 0.3963 0.1182 0.4425 0.026 Uiso 1 1 calc R
H1W1 H 0.694(3) 0.039(3) 0.850(2) 0.024(8) Uiso 1 1 d D
H2W1 H 0.483(3) 0.061(3) 0.826(3) 0.037(9) Uiso 1 1 d D
H2W2 H 0.063(5) 0.135(3) 0.892(2) 0.044(10) Uiso 1 1 d D
H1W2 H 0.076(5) 0.176(4) 1.0055(15) 0.048(11) Uiso 1 1 d D
H1W4 H 0.578(4) 0.201(3) 1.0976(18) 0.034(9) Uiso 1 1 d D
H2W4 H 0.538(5) 0.197(4) 0.9813(18) 0.044(10) Uiso 1 1 d D
H1W5 H 0.285(4) 0.367(2) 0.886(3) 0.044(10) Uiso 1 1 d D
H2W5 H 0.273(4) 0.543(3) 0.844(2) 0.037(9) Uiso 1 1 d D
H2W3 H 0.150(4) 0.440(2) 1.134(2) 0.035(9) Uiso 1 1 d D
H1W3 H 0.127(4) 0.617(2) 1.091(2) 0.022(8) Uiso 1 1 d 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'
Ni Ni 0.3393 1.1124 '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
OW4 Ni1 OW4 180.000(1) . 2_667
OW4 Ni1 OW5 88.03(7) . .
OW4 Ni1 OW5 91.97(7) 2_667 .
OW4 Ni1 OW5 91.97(7) . 2_667
OW4 Ni1 OW5 88.03(7) 2_667 2_667
OW5 Ni1 OW5 180.000(1) . 2_667
OW4 Ni1 OW3 90.01(7) . 2_667
OW4 Ni1 OW3 89.99(7) 2_667 2_667
OW5 Ni1 OW3 87.60(7) . 2_667
OW5 Ni1 OW3 92.40(7) 2_667 2_667
OW4 Ni1 OW3 89.99(7) . .
OW4 Ni1 OW3 90.01(7) 2_667 .
OW5 Ni1 OW3 92.40(7) . .
OW5 Ni1 OW3 87.60(7) 2_667 .
OW3 Ni1 OW3 180.0 2_667 .
O3 S1 O3 0.00(18) 1 .
O3 S1 O4 110.83(10) 1 .
O3 S1 O4 110.83(10) . .
O3 S1 O2 110.23(10) 1 1
O3 S1 O2 110.23(10) . 1
O4 S1 O2 109.23(10) . 1
O3 S1 O2 110.23(10) 1 .
O3 S1 O2 110.23(10) . .
O4 S1 O2 109.23(10) . .
O2 S1 O2 0.00(13) 1 .
O3 S1 O1 109.07(10) 1 .
O3 S1 O1 109.07(10) . .
O4 S1 O1 108.69(10) . .
O2 S1 O1 108.75(10) 1 .
O2 S1 O1 108.75(10) . .
O2 O2 S1 0(10) 1 .
H1W1 OW1 H2W1 109(2) . .
Ni1 OW4 H1W4 124.9(19) . .
Ni1 OW4 H2W4 110.6(19) . .
H1W4 OW4 H2W4 105(2) . .
O3 O3 S1 0(10) 1 .
Ni1 OW5 H1W5 111(2) . .
Ni1 OW5 H2W5 116.5(19) . .
H1W5 OW5 H2W5 106(2) . .
H2W2 OW2 H1W2 104(2) . .
C6 C5 C4 121.5(2) . .
C6 C5 H5 119.3 . .
C4 C5 H5 119.3 . .
Ni1 OW3 H2W3 118.1(18) . .
Ni1 OW3 H1W3 121.0(17) . .
H2W3 OW3 H1W3 110(2) . .
C1 N2 C2 109.0(2) . .
C1 N2 HN2 125.5 . .
C2 N2 HN2 125.5 . .
N1 C1 N2 110.0(2) . .
N1 C1 H1 125.0 . .
N2 C1 H1 125.0 . .
C1 N1 C7 108.8(2) . .
C1 N1 HN1 125.6 . .
C7 N1 HN1 125.6 . .
C4 C3 C2 116.5(2) . .
C4 C3 H3 121.7 . .
C2 C3 H3 121.7 . .
C3 C2 N2 132.4(2) . .
C3 C2 C7 121.8(2) . .
N2 C2 C7 105.8(2) . .
N1 C7 C2 106.4(2) . .
N1 C7 C6 132.1(2) . .
C2 C7 C6 121.6(2) . .
C5 C6 C7 116.4(2) . .
C5 C6 H6 121.8 . .
C7 C6 H6 121.8 . .
C3 C4 C5 122.3(2) . .
C3 C4 H4 118.9 . .
C5 C4 H4 118.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 OW4 2.0261(17) .
Ni1 OW4 2.0261(17) 2_667
Ni1 OW5 2.0686(17) .
Ni1 OW5 2.0686(17) 2_667
Ni1 OW3 2.0789(16) 2_667
Ni1 OW3 2.0789(16) .
S1 O3 1.4680(18) 1
S1 O3 1.4680(18) .
S1 O4 1.4733(17) .
S1 O2 1.4798(17) 1
S1 O2 1.4798(17) .
S1 O1 1.4872(17) .
O2 O2 0.000(5) 1
OW1 H1W1 0.898(16) .
OW1 H2W1 0.929(17) .
OW4 H1W4 0.951(17) .
OW4 H2W4 0.944(17) .
O3 O3 0.000(5) 1
OW5 H1W5 0.913(17) .
OW5 H2W5 0.950(17) .
OW2 H2W2 0.938(17) .
OW2 H1W2 0.943(17) .
C5 C6 1.380(4) .
C5 C4 1.403(4) .
C5 H5 0.9300 .
OW3 H2W3 0.917(17) .
OW3 H1W3 0.922(16) .
N2 C1 1.322(3) .
N2 C2 1.389(3) .
N2 HN2 0.8600 .
C1 N1 1.320(3) .
C1 H1 0.9300 .
N1 C7 1.388(3) .
N1 HN1 0.8600 .
C3 C4 1.371(4) .
C3 C2 1.388(4) .
C3 H3 0.9300 .
C2 C7 1.394(3) .
C7 C6 1.397(3) .
C6 H6 0.9300 .
C4 H4 0.9300 .
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
OW4 H1W4 O4 0.951(17) 1.792(17) 2.737(2) 172(3) 2_667
OW5 H2W5 O2 0.950(17) 1.752(18) 2.696(2) 172(3) 1
OW3 H2W3 O2 0.917(17) 1.90(2) 2.762(2) 156(2) 2_567
OW1 H1W1 O1 0.898(16) 1.844(17) 2.714(2) 163(3) 1_645
OW1 H2W1 O4 0.929(17) 1.95(2) 2.844(2) 162(3) 1_545
OW2 H2W2 O1 0.938(17) 1.86(2) 2.746(2) 157(3) 1_545
OW2 H1W2 O1 0.943(17) 1.872(19) 2.801(2) 168(3) 2_567
N2 HN2 OW1 0.86 2.31 2.913(3) 127.1 2_666
N1 HN1 O3 0.86 1.86 2.711(3) 170.1 1
