#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:59:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179874 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/70/7017059.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_7017059
loop_
_publ_author_name
'Hajlaoui, Fadhel'
'Naïli, Houcine'
'Yahyaoui, Samia'
'Turnbull, Mark M.'
'Mhiri, Tahar'
'Bataille, Thierry'
_publ_section_title
;
 Synthesis, characterization and magnetic properties of four new
 organically templated metal sulfates
 [C(5)H(14)N(2)][M(II)(H(2)O)(6)](SO(4))(2), (M(II) = Mn, Fe, Co, Ni).
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11613
_journal_page_last               11620
_journal_paper_doi               10.1039/c1dt11030f
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C5 H26 N2 Ni O14 S2'
_chemical_formula_weight         461.11
_chemical_name_systematic
;
?
;
_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                 116.8260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8328(2)
_cell_length_b                   7.84430(10)
_cell_length_c                   11.6790(2)
_cell_measurement_temperature    293(2)
_cell_volume                     885.63(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1033
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10356
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.25
_exptl_absorpt_coefficient_mu    1.401
_exptl_absorpt_correction_T_max  0.7624
_exptl_absorpt_correction_T_min  0.4936
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.034(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2012
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0414
_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)+(0.0366P)²+2.0088P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                1955
_reflns_number_total             2012
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11030f.txt
_cod_data_source_block           (Ni)import
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Analytical'
changed to 'analytical' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        885.63(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7017059
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
Ni1 Ni 0.0000 0.5000 0.0000 0.0236(2) Uani 1 2 d S
OW1 O -0.2099(2) 0.5306(3) -0.1126(2) 0.0310(5) Uani 1 1 d D
OW2 O -0.0398(3) 0.5487(3) 0.1539(2) 0.0332(5) Uani 1 1 d D
OW3 O -0.0214(2) 0.2438(3) 0.0235(3) 0.0369(5) Uani 1 1 d D
S1 S 0.25860(7) 1.06282(9) -0.04359(7) 0.0253(2) Uani 1 1 d .
O1 O 0.3290(2) 1.1929(3) 0.0553(2) 0.0358(5) Uani 1 1 d .
O2 O 0.1094(2) 1.1085(3) -0.1160(2) 0.0330(5) Uani 1 1 d .
O3 O 0.3238(3) 1.0537(4) -0.1293(2) 0.0412(6) Uani 1 1 d .
O4 O 0.2682(3) 0.8955(3) 0.0161(3) 0.0459(7) Uani 1 1 d .
N1 N 0.4557(3) 0.6721(4) -0.0024(4) 0.0543(10) Uani 1 1 d .
H1A H 0.5172 0.7288 -0.0203 0.065 Uiso 1 1 calc R
H1B H 0.3979 0.7492 0.0047 0.065 Uiso 1 1 calc R
C1 C 0.3045(9) 0.6370(10) -0.2157(6) 0.0463(18) Uani 0.50 1 d P
H1C H 0.2461 0.7184 -0.2023 0.069 Uiso 0.50 1 calc PR
H1D H 0.2485 0.5599 -0.2830 0.069 Uiso 0.50 1 calc PR
H1E H 0.3674 0.6956 -0.2393 0.069 Uiso 0.50 1 calc PR
C2 C 0.3742(4) 0.5518(5) -0.1106(5) 0.0594(13) Uani 1 1 d .
H2 H 0.3075 0.4928 -0.0893 0.071 Uiso 1 1 calc R
C3 C 0.5296(4) 0.5817(5) 0.1204(5) 0.0562(12) Uani 1 1 d .
H3A H 0.4633 0.5272 0.1431 0.067 Uiso 1 1 calc R
H3B H 0.5828 0.6626 0.1874 0.067 Uiso 1 1 calc R
HW1 H -0.242(6) 0.533(6) -0.203(2) 0.073(17) Uiso 1 1 d D
HW2 H -0.237(4) 0.637(4) -0.092(3) 0.051(12) Uiso 1 1 d D
HW3 H -0.059(5) 0.660(3) 0.168(4) 0.064(14) Uiso 1 1 d D
HW4 H 0.015(6) 0.499(6) 0.234(3) 0.09(2) Uiso 1 1 d D
HW5 H -0.109(3) 0.205(6) 0.009(4) 0.058(13) Uiso 1 1 d D
HW6 H 0.007(6) 0.180(9) -0.028(6) 0.16(3) 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
OW3 Ni1 OW3 180.0 . 3_565
OW3 Ni1 OW1 87.67(9) . 3_565
OW3 Ni1 OW1 92.33(9) 3_565 3_565
OW3 Ni1 OW1 92.33(9) . .
OW3 Ni1 OW1 87.67(9) 3_565 .
OW1 Ni1 OW1 180.0 3_565 .
OW3 Ni1 OW2 89.11(10) . .
OW3 Ni1 OW2 90.89(10) 3_565 .
OW1 Ni1 OW2 94.02(9) 3_565 .
OW1 Ni1 OW2 85.98(9) . .
OW3 Ni1 OW2 90.89(10) . 3_565
OW3 Ni1 OW2 89.11(10) 3_565 3_565
OW1 Ni1 OW2 85.98(9) 3_565 3_565
OW1 Ni1 OW2 94.02(9) . 3_565
OW2 Ni1 OW2 180.0 . 3_565
Ni1 OW1 HW1 117(3) . .
Ni1 OW1 HW2 109(3) . .
HW1 OW1 HW2 105(2) . .
Ni1 OW2 HW3 119(3) . .
Ni1 OW2 HW4 120(4) . .
HW3 OW2 HW4 108(3) . .
Ni1 OW3 HW5 117(3) . .
Ni1 OW3 HW6 110(5) . .
HW5 OW3 HW6 108(3) . .
O3 S1 O4 109.15(16) . 1
O3 S1 O4 109.15(16) . .
O4 S1 O4 0.0(2) 1 .
O3 S1 O1 109.39(14) . .
O4 S1 O1 110.32(16) 1 .
O4 S1 O1 110.32(16) . .
O3 S1 O2 110.97(15) . .
O4 S1 O2 108.10(14) 1 .
O4 S1 O2 108.10(14) . .
O1 S1 O2 108.91(13) . .
O4 O4 S1 0(10) 1 .
C3 N1 C2 111.8(3) . .
C3 N1 H1A 109.3 . .
C2 N1 H1A 109.3 . .
C3 N1 H1B 109.3 . .
C2 N1 H1B 109.3 . .
H1A N1 H1B 107.9 . .
C2 C1 H1C 109.5 . .
C2 C1 H1D 109.5 . .
H1C C1 H1D 109.5 . .
C2 C1 H1E 109.5 . .
H1C C1 H1E 109.5 . .
H1D C1 H1E 109.5 . .
C1 C2 N1 110.0(5) . .
C1 C2 C3 114.2(6) . 3_665
N1 C2 C3 109.5(3) . 3_665
C1 C2 H2 107.6 . .
N1 C2 H2 107.6 . .
C3 C2 H2 107.6 3_665 .
N1 C3 C2 110.5(4) . 3_665
N1 C3 H3A 109.5 . .
C2 C3 H3A 109.5 3_665 .
N1 C3 H3B 109.5 . .
C2 C3 H3B 109.5 3_665 .
H3A C3 H3B 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 OW3 2.056(2) .
Ni1 OW3 2.056(2) 3_565
Ni1 OW1 2.064(2) 3_565
Ni1 OW1 2.064(2) .
Ni1 OW2 2.065(2) .
Ni1 OW2 2.065(2) 3_565
OW1 HW1 0.951(19) .
OW1 HW2 0.948(18) .
OW2 HW3 0.929(19) .
OW2 HW4 0.940(19) .
OW3 HW5 0.937(19) .
OW3 HW6 0.94(2) .
S1 O3 1.464(2) .
S1 O4 1.468(2) 1
S1 O4 1.468(2) .
S1 O1 1.471(2) .
S1 O2 1.490(2) .
O4 O4 0.000(8) 1
N1 C3 1.471(6) .
N1 C2 1.504(5) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
C1 C2 1.298(8) .
C1 H1C 0.9600 .
C1 H1D 0.9600 .
C1 H1E 0.9600 .
C2 C3 1.517(5) 3_665
C2 H2 0.9800 .
C3 C2 1.517(5) 3_665
C3 H3A 0.9700 .
C3 H3B 0.9700 .
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
OW1 HW1 O3 0.951(19) 1.76(2) 2.700(3) 171(5) 2_544
OW1 HW2 O1 0.948(18) 1.83(2) 2.755(3) 164(4) 3_575
OW2 HW3 O2 0.929(19) 1.92(2) 2.774(3) 153(4) 3_575
OW2 HW4 O2 0.940(19) 1.789(19) 2.726(3) 175(6) 4_576
OW3 HW5 O4 0.937(19) 1.80(2) 2.728(3) 173(4) 3_565
OW3 HW6 O2 0.94(2) 1.90(2) 2.805(3) 161(5) 1_545
N1 H1A O1 0.90 1.98 2.871(4) 168.2 3_675
N1 H1B O4 0.90 1.87 2.763(4) 175.6 1
