#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:59:43 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179874 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/70/7017057.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_7017057
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 Fe N2 O14 S2'
_chemical_formula_weight         458.25
_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                 116.7330(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.9273(2)
_cell_length_b                   7.86200(10)
_cell_length_c                   11.7845(3)
_cell_measurement_temperature    293(2)
_cell_volume                     904.20(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13422
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.8767
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   analytical
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2750
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0431
_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)+(0.0506P)²+0.7368P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                2290
_reflns_number_total             2750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11030f.txt
_cod_data_source_block           (Fe)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_sg_symbol_H-M      P21/c
_cod_database_code               7017057
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
Fe1 Fe 0.0000 0.5000 0.0000 0.02925(15) Uani 1 2 d S
OW1 O -0.02937(19) 0.2377(2) 0.0132(2) 0.0495(5) Uani 1 1 d D
OW2 O -0.04161(18) 0.5455(2) 0.15836(17) 0.0410(4) Uani 1 1 d D
OW3 O 0.21285(17) 0.4604(2) 0.11682(17) 0.0400(4) Uani 1 1 d D
S1 S 0.26175(5) 1.06371(6) -0.04318(5) 0.02990(15) Uani 1 1 d .
O1 O 0.11505(16) 1.1114(2) -0.11481(17) 0.0386(4) Uani 1 1 d .
O2 O 0.32718(18) 1.0548(3) -0.12764(18) 0.0465(4) Uani 1 1 d .
O3 O 0.33231(16) 1.1920(2) 0.05550(17) 0.0412(4) Uani 1 1 d .
O4 O 0.27001(19) 0.8961(2) 0.0151(2) 0.0517(5) Uani 1 1 d .
N1 N 0.4551(2) 0.6713(3) -0.0033(3) 0.0599(8) Uani 1 1 d .
H1A H 0.5166 0.7284 -0.0199 0.072 Uiso 1 1 calc R
H1B H 0.3967 0.7477 0.0024 0.072 Uiso 1 1 calc R
C1 C 0.3771(3) 0.5510(4) -0.1102(4) 0.0638(10) Uani 1 1 d .
H1 H 0.3092 0.4925 -0.0914 0.077 Uiso 1 1 calc R
C2 C 0.5268(3) 0.5820(4) 0.1186(4) 0.0637(9) Uani 1 1 d .
H2A H 0.4604 0.5276 0.1403 0.076 Uiso 1 1 calc R
H2B H 0.5786 0.6630 0.1850 0.076 Uiso 1 1 calc R
C3 C 0.3121(6) 0.6367(6) -0.2141(4) 0.0536(14) Uani 0.50 1 d P
H3A H 0.2534 0.7185 -0.2027 0.080 Uiso 0.50 1 calc PR
H3B H 0.2579 0.5605 -0.2819 0.080 Uiso 0.50 1 calc PR
H3C H 0.3768 0.6945 -0.2348 0.080 Uiso 0.50 1 calc PR
HW6 H 0.2453 0.3605 0.0942 0.075(11) Uiso 1 1 d RD
HW3 H 0.0043 0.5031 0.2410 0.065(11) Uiso 1 1 d RD
HW2 H -0.1159 0.1910 -0.0037 0.097(14) Uiso 1 1 d RD
HW5 H 0.2496 0.4555 0.2063 0.062(10) Uiso 1 1 d RD
HW1 H 0.0061 0.1699 -0.0311 0.112(16) Uiso 1 1 d RD
HW4 H -0.0664 0.6580 0.1651 0.090(13) Uiso 1 1 d RD
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'
Fe Fe 0.3463 0.8444 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
OW1 Fe1 OW1 180.0 3_565 .
OW1 Fe1 OW3 91.87(7) 3_565 .
OW1 Fe1 OW3 88.13(7) . .
OW1 Fe1 OW3 88.13(7) 3_565 3_565
OW1 Fe1 OW3 91.87(7) . 3_565
OW3 Fe1 OW3 180.0 . 3_565
OW1 Fe1 OW2 90.01(7) 3_565 3_565
OW1 Fe1 OW2 89.99(7) . 3_565
OW3 Fe1 OW2 86.59(7) . 3_565
OW3 Fe1 OW2 93.41(7) 3_565 3_565
OW1 Fe1 OW2 89.99(7) 3_565 .
OW1 Fe1 OW2 90.01(7) . .
OW3 Fe1 OW2 93.41(7) . .
OW3 Fe1 OW2 86.59(7) 3_565 .
OW2 Fe1 OW2 180.00(13) 3_565 .
Fe1 OW1 HW2 122.4 . .
Fe1 OW1 HW1 113.5 . .
HW2 OW1 HW1 106.5 . .
Fe1 OW2 HW3 128.7 . .
Fe1 OW2 HW4 114.5 . .
HW3 OW2 HW4 106.7 . .
Fe1 OW3 HW6 112.2 . .
Fe1 OW3 HW5 121.3 . .
HW6 OW3 HW5 104.8 . .
O2 S1 O3 109.15(10) . .
O2 S1 O4 109.15(12) . .
O3 S1 O4 110.23(12) . .
O2 S1 O1 110.97(11) . .
O3 S1 O1 108.95(9) . .
O4 S1 O1 108.39(10) . .
C2 N1 C1 111.8(2) . .
C2 N1 H1A 109.3 . .
C1 N1 H1A 109.3 . .
C2 N1 H1B 109.3 . .
C1 N1 H1B 109.3 . .
H1A N1 H1B 107.9 . .
C3 C1 N1 109.2(3) . .
C3 C1 C2 113.5(4) . 3_665
N1 C1 C2 110.0(2) . 3_665
C3 C1 H1 108.0 . .
N1 C1 H1 108.0 . .
C2 C1 H1 108.0 3_665 .
N1 C2 C1 110.2(3) . 3_665
N1 C2 H2A 109.6 . .
C1 C2 H2A 109.6 3_665 .
N1 C2 H2B 109.6 . .
C1 C2 H2B 109.6 3_665 .
H2A C2 H2B 108.1 . .
C1 C3 H3A 109.5 . .
C1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 OW1 2.1036(16) 3_565
Fe1 OW1 2.1036(16) .
Fe1 OW3 2.1263(16) .
Fe1 OW3 2.1263(16) 3_565
Fe1 OW2 2.1403(17) 3_565
Fe1 OW2 2.1403(17) .
OW1 HW2 0.9483 .
OW1 HW1 0.9423 .
OW2 HW3 0.9331 .
OW2 HW4 0.9394 .
OW3 HW6 0.9473 .
OW3 HW5 0.9454 .
S1 O2 1.4652(18) .
S1 O3 1.4689(16) .
S1 O4 1.4696(17) .
S1 O1 1.4850(16) .
N1 C2 1.469(5) .
N1 C1 1.498(4) .
N1 H1A 0.9000 .
N1 H1B 0.9000 .
C1 C3 1.294(6) .
C1 C2 1.516(4) 3_665
C1 H1 0.9800 .
C2 C1 1.516(4) 3_665
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
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
N1 H1A O3 0.90 1.98 2.866(3) 168.4 3_675
N1 H1B O4 0.90 1.87 2.767(3) 176.9 .
OW3 HW6 O3 0.95 1.81 2.743(2) 170.2 1_545
OW2 HW3 O1 0.93 1.82 2.735(2) 166.0 4_576
OW1 HW2 O4 0.95 1.77 2.710(2) 173.1 3_565
OW3 HW5 O2 0.95 1.75 2.694(3) 176.6 4_576
OW1 HW1 O1 0.94 1.91 2.810(2) 158.1 1_545
OW2 HW4 O1 0.94 1.91 2.796(2) 156.9 3_575
OW3 HW6 O3 0.95 1.81 2.743(2) 170.2 1_545
