#------------------------------------------------------------------------------
#$Date: 2016-02-20 21:30:07 +0100 (Sat 20 de Feb de 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/13/2221357.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_2221357
loop_
_publ_author_name
'Peterson, Larnelle'
'Kelley, Jennifer'
'Peterson, Jr, LeRoy'
'Smith, Mark D.'
'Loye, Hans-Conrad zur'
_publ_section_title
;
 Tetraquabis(5-fluorosaccharinato)nickel(II)
;
_journal_coeditor_code           HB2907
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m364
_journal_page_last               m365
_journal_paper_doi               10.1107/S1600536809007053
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Ni (C7 H3 F N O3 S)2 (H2 O)4]'
_chemical_formula_moiety         'C14 H14 F2 N2 Ni O10 S2'
_chemical_formula_sum            'C14 H14 F2 N2 Ni O10 S2'
_chemical_formula_weight         531.10
_chemical_name_systematic
;
Tetraquabis(5-fluorosaccharinato)nickel(II)
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.7800(10)
_cell_angle_beta                 105.9830(10)
_cell_angle_gamma                110.9730(10)
_cell_formula_units_Z            1
_cell_length_a                   6.9649(3)
_cell_length_b                   8.0484(3)
_cell_length_c                   9.5877(4)
_cell_measurement_reflns_used    4507
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.390
_cell_measurement_theta_min      2.347
_cell_volume                     454.19(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2003)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2005)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_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  0.0224
_diffrn_reflns_av_sigmaI/netI    0.0199
_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       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6861
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    1.381
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2003)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             270
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.375
_refine_diff_density_min         -0.367
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         1858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0244
_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)+(0.0376P)²+0.2342P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0653
_reflns_number_gt                1769
_reflns_number_total             1858
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb2907.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        454.18(3)
_cod_database_code               2221357
_cod_database_fobs_code          2221357
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.5000 0.5000 0.5000 0.01450(11) Uani d S 1 . .
S S1 -0.01342(6) 0.32955(6) 0.24583(5) 0.01495(12) Uani d . 1 . .
C C1 0.2752(3) 0.2997(2) 0.1523(2) 0.0176(4) Uani d . 1 . .
C C2 0.0749(3) 0.2377(2) 0.0098(2) 0.0164(3) Uani d . 1 . .
C C3 0.0542(3) 0.1736(2) -0.1416(2) 0.0179(3) Uani d . 1 . .
H H3 0.1724 0.1621 -0.1670 0.020(5) Uiso calc R 1 . .
C C4 -0.1482(3) 0.1274(2) -0.2531(2) 0.0179(3) Uani d . 1 . .
C C5 -0.3263(3) 0.1414(3) -0.2223(2) 0.0217(4) Uani d . 1 . .
H H5 -0.4613 0.1090 -0.3041 0.036(6) Uiso calc R 1 . .
C C6 -0.3043(3) 0.2036(3) -0.0695(2) 0.0209(4) Uani d . 1 . .
H H6 -0.4232 0.2132 -0.0438 0.026(6) Uiso calc R 1 . .
C C7 -0.1013(3) 0.2507(2) 0.04337(19) 0.0169(3) Uani d . 1 . .
F F1 -0.17280(17) 0.06728(16) -0.40248(12) 0.0230(2) Uani d . 1 . .
N N1 0.2420(2) 0.3605(2) 0.28345(17) 0.0172(3) Uani d . 1 . .
O O1 0.4490(2) 0.2954(2) 0.15047(15) 0.0258(3) Uani d . 1 . .
O O2 -0.1302(2) 0.18308(18) 0.29833(15) 0.0210(3) Uani d . 1 . .
O O3 -0.01877(19) 0.50819(17) 0.30498(14) 0.0193(3) Uani d . 1 . .
O O4 0.2988(2) 0.3398(2) 0.59836(16) 0.0197(3) Uani d . 1 . .
H H4A 0.190(5) 0.249(4) 0.535(4) 0.048(8) Uiso d . 1 . .
H H4B 0.254(5) 0.396(4) 0.646(3) 0.043(8) Uiso d . 1 . .
O O5 0.4047(2) 0.71025(18) 0.54925(17) 0.0187(3) Uani d . 1 . .
H H5A 0.284(5) 0.685(4) 0.490(3) 0.046(8) Uiso d . 1 . .
H H5B 0.412(4) 0.742(4) 0.637(3) 0.039(7) 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'
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'
F F 0.0171 0.0103 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O5 Ni1 O5 2_666 . 180.0 n
O5 Ni1 N1 2_666 . 87.50(6) n
O5 Ni1 N1 . . 92.50(6) ?
O5 Ni1 N1 2_666 2_666 92.50(6) ?
O5 Ni1 N1 . 2_666 87.50(6) ?
N1 Ni1 N1 . 2_666 180.0 n
O5 Ni1 O4 2_666 . 88.53(5) n
O5 Ni1 O4 . . 91.47(5) ?
N1 Ni1 O4 . . 90.65(6) ?
N1 Ni1 O4 2_666 . 89.35(6) ?
O5 Ni1 O4 2_666 2_666 91.47(5) ?
O5 Ni1 O4 . 2_666 88.53(5) ?
N1 Ni1 O4 . 2_666 89.35(6) ?
N1 Ni1 O4 2_666 2_666 90.65(6) n
O4 Ni1 O4 . 2_666 180.0 n
O2 S1 O3 . . 114.08(7) ?
O2 S1 N1 . . 110.96(8) ?
O3 S1 N1 . . 110.42(7) ?
O2 S1 C7 . . 111.32(8) ?
O3 S1 C7 . . 112.14(8) ?
N1 S1 C7 . . 96.63(8) ?
O1 C1 N1 . . 124.25(16) ?
O1 C1 C2 . . 123.43(16) ?
N1 C1 C2 . . 112.32(14) ?
C7 C2 C3 . . 120.66(16) ?
C7 C2 C1 . . 112.04(15) ?
C3 C2 C1 . . 127.30(15) ?
C4 C3 C2 . . 116.09(15) ?
C4 C3 H3 . . 122.0 ?
C2 C3 H3 . . 122.0 ?
F1 C4 C3 . . 117.60(15) ?
F1 C4 C5 . . 118.11(16) ?
C3 C4 C5 . . 124.28(17) ?
C4 C5 C6 . . 119.03(16) ?
C4 C5 H5 . . 120.5 ?
C6 C5 H5 . . 120.5 ?
C7 C6 C5 . . 117.06(16) ?
C7 C6 H6 . . 121.5 ?
C5 C6 H6 . . 121.5 ?
C2 C7 C6 . . 122.86(16) ?
C2 C7 S1 . . 107.03(13) ?
C6 C7 S1 . . 130.10(13) ?
C1 N1 S1 . . 111.66(12) ?
C1 N1 Ni1 . . 122.66(11) ?
S1 N1 Ni1 . . 125.40(8) ?
Ni1 O4 H4A . . 113(2) ?
Ni1 O4 H4B . . 113(2) ?
H4A O4 H4B . . 106(3) ?
Ni1 O5 H5A . . 113(2) ?
Ni1 O5 H5B . . 113.5(19) ?
H5A O5 H5B . . 110(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 O5 2_666 2.0440(13) n
Ni1 O5 . 2.0440(13) y
Ni1 N1 . 2.0856(14) yes
Ni1 N1 2_666 2.0856(14) ?
Ni1 O4 . 2.1084(13) yes
Ni1 O4 2_666 2.1084(13) ?
S1 O2 . 1.4443(13) ?
S1 O3 . 1.4515(13) ?
S1 N1 . 1.6277(14) ?
S1 C7 . 1.7635(17) ?
C1 O1 . 1.228(2) ?
C1 N1 . 1.366(2) ?
C1 C2 . 1.495(2) ?
C2 C7 . 1.385(2) ?
C2 C3 . 1.385(2) ?
C3 C4 . 1.379(2) ?
C3 H3 . 0.9500 ?
C4 F1 . 1.355(2) ?
C4 C5 . 1.388(2) ?
C5 C6 . 1.394(3) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.385(2) ?
C6 H6 . 0.9500 ?
O4 H4A . 0.81(3) ?
O4 H4B . 0.78(3) ?
O5 H5A . 0.80(3) ?
O5 H5B . 0.81(3) ?
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
O4 H4A O2 . 0.81(3) 2.51(3) 3.1436(19) 137(3)
O4 H4A F1 2 0.81(3) 2.54(3) 3.0910(19) 127(3)
O4 H4B O3 2_566 0.78(3) 2.17(3) 2.8985(18) 158(3)
O5 H5A O3 . 0.80(3) 2.10(3) 2.8346(18) 155(3)
O5 H5A F1 2_565 0.80(3) 2.59(3) 3.1050(17) 124(2)
O5 H5B O1 2_666 0.81(3) 2.13(3) 2.793(2) 139(2)
O5 H5B O2 2_566 0.81(3) 2.44(3) 2.9541(18) 122(2)
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1 C1 C2 C7 . . . . 177.99(17) ?
N1 C1 C2 C7 . . . . -1.9(2) ?
O1 C1 C2 C3 . . . . -2.1(3) ?
N1 C1 C2 C3 . . . . 178.04(16) ?
C7 C2 C3 C4 . . . . 0.8(3) ?
C1 C2 C3 C4 . . . . -179.07(16) ?
C2 C3 C4 F1 . . . . 178.87(14) ?
C2 C3 C4 C5 . . . . 0.0(3) ?
F1 C4 C5 C6 . . . . -179.76(16) ?
C3 C4 C5 C6 . . . . -0.9(3) ?
C4 C5 C6 C7 . . . . 0.9(3) ?
C3 C2 C7 C6 . . . . -0.7(3) ?
C1 C2 C7 C6 . . . . 179.18(16) ?
C3 C2 C7 S1 . . . . 178.11(14) ?
C1 C2 C7 S1 . . . . -1.98(18) ?
C5 C6 C7 C2 . . . . -0.2(3) ?
C5 C6 C7 S1 . . . . -178.74(14) ?
O2 S1 C7 C2 . . . . -111.27(13) ?
O3 S1 C7 C2 . . . . 119.56(12) ?
N1 S1 C7 C2 . . . . 4.32(14) ?
O2 S1 C7 C6 . . . . 67.46(19) ?
O3 S1 C7 C6 . . . . -61.72(19) ?
N1 S1 C7 C6 . . . . -176.96(18) ?
O1 C1 N1 S1 . . . . -174.70(15) ?
C2 C1 N1 S1 . . . . 5.15(19) ?
O1 C1 N1 Ni1 . . . . 11.1(3) ?
C2 C1 N1 Ni1 . . . . -169.10(11) ?
O2 S1 N1 C1 . . . . 110.32(13) ?
O3 S1 N1 C1 . . . . -122.18(13) ?
C7 S1 N1 C1 . . . . -5.56(14) ?
O2 S1 N1 Ni1 . . . . -75.62(11) ?
O3 S1 N1 Ni1 . . . . 51.87(12) ?
C7 S1 N1 Ni1 . . . . 168.50(10) ?
O5 Ni1 N1 C1 2_666 . . . -48.82(14) ?
O5 Ni1 N1 C1 . . . . 131.18(14) ?
O4 Ni1 N1 C1 . . . . -137.32(14) ?
O4 Ni1 N1 C1 2_666 . . . 42.68(14) ?
O5 Ni1 N1 S1 2_666 . . . 137.74(10) ?
O5 Ni1 N1 S1 . . . . -42.26(10) ?
O4 Ni1 N1 S1 . . . . 49.24(10) ?
O4 Ni1 N1 S1 2_666 . . . -130.76(10) ?
