#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/24/2202450.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_2202450
loop_
_publ_author_name
'Wu, Bei'
'Taylor, Max R.'
'Martin, Lisandra L.'
_publ_section_title
;
 Aquabis(4-morpholinyldithiocarbamato)iron(III)
 trifluoromethanesulfonate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1083
_journal_page_last               m1085
_journal_paper_doi               10.1107/S1600536803024462
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Fe (C5 H8 N O S2)2 (H2 O)] C F3 S O3'
_chemical_formula_moiety         'C10 H18 Fe N2 O3 S4 1+, C F3 O3 S 1-'
_chemical_formula_sum            'C11 H18 F3 Fe N2 O6 S5'
_chemical_formula_weight         547.44
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   18.929(6)
_cell_length_b                   10.197(3)
_cell_length_c                   11.214(4)
_cell_measurement_reflns_used    7138
_cell_measurement_temperature    168
_cell_measurement_theta_max      26.07
_cell_measurement_theta_min      2.11
_cell_volume                     2164.5(12)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction
'SAINT (Bruker, 2000) and Xtal3.7 ADDREF and SORTRF (Hall et al., 2000)'
_computing_molecular_graphics    Xtal3.7
_computing_publication_material  'Xtal3.7 BONDLA and CIFIO'
_computing_structure_refinement  'Xtal3.7 CRYLSQ'
_computing_structure_solution    'SIR97 (Altomare et al., 1994)'
_diffrn_ambient_temperature      168
_diffrn_measured_fraction_theta_full .99
_diffrn_measured_fraction_theta_max .99
_diffrn_measurement_device_type
;
Bruker SMART CCD area-detector
;
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fixed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .059
_diffrn_reflns_av_sigmaI/netI    .039
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26787
_diffrn_reflns_theta_full        26.38
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.829
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.68
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1116
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         .94
_refine_diff_density_min         -.61
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   .989
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2157
_refine_ls_number_restraints     17
_refine_ls_R_factor_all          .067
_refine_ls_R_factor_gt           .042
_refine_ls_shift/su_max          .018
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fₒ²) + (0.03Fₒ²)²]^1/2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .096
_refine_ls_wR_factor_ref         .094
_reflns_number_gt                1677
_reflns_number_total             2316
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cf6293.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     -p_2ac_2n
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'C11 H18 F3 Fe1 N2 O6 S5'
_cod_database_code               2202450
_cod_database_fobs_code          2202450
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
1/2-x,-y,1/2+z
1/2+x,1/2-y,1/2-z
-x,1/2+y,-z
-x,-y,-z
1/2+x,+y,1/2-z
1/2-x,1/2+y,1/2+z
+x,1/2-y,+z
loop_
_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_calc_attached_atom
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
F7a .1315(4) .2921(4) -.1701(4) .167(10) Uani ? ? .50000 ? ?
F7b .0406(3) .3296(6) -.0597(6) .188(11) Uani ? ? .50000 ? ?
F7c .0700(4) .1314(4) -.1009(7) .130(8) Uani ? ? .50000 ? ?
C7 .0950(3) .25000 -.0772(4) .079(7) Uani ? ? 1.00000 ? ?
O3a .1703(2) .3812(2) .0635(3) .117(8) Uani ? ? .50000 ? ?
O3b .1061(2) .1924(4) .1426(3) .089(5) Uani ? ? .50000 ? ?
O3c .2043(3) .1594(4) .0107(6) .072(5) Uani ? ? .50000 ? ?
S3 .14978(8) .25000 .05120(14) .0447(9) Uani ? ? 1.00000 ? ?
Fe .07070(3) .25000 .48871(6) .0219(4) Uani ? ? 1.00000 ? ?
S1 .16273(5) .38901(8) .45124(8) .0262(5) Uani ? ? 1.00000 ? ?
S2 .00247(5) .38877(9) .60008(8) .0268(5) Uani ? ? 1.00000 ? ?
N1 .2750(2) .25000 .3714(4) .026(2) Uani ? ? 1.00000 ? ?
N2 -.0819(2) .25000 .7474(3) .025(2) Uani ? ? 1.00000 ? ?
O1 .3858(2) .25000 .2041(3) .042(2) Uani ? ? 1.00000 ? ?
O2 -.2175(2) .25000 .8529(4) .042(2) Uani ? ? 1.00000 ? ?
O3 .02481(18) .25000 .3267(3) .039(2) Uani ? ? 1.00000 ? ?
C1 .2108(3) .25000 .4170(4) .023(3) Uani ? ? 1.00000 ? ?
C2 .31528(19) .3698(4) .3486(3) .032(2) Uani ? ? 1.00000 ? ?
C3 .3443(2) .3658(4) .2209(4) .038(2) Uani ? ? 1.00000 ? ?
C4 -.0341(3) .25000 .6630(4) .022(3) Uani ? ? 1.00000 ? ?
C5 -.1116(2) .3709(3) .7993(3) .031(2) Uani ? ? 1.00000 ? ?
C6 -.1918(2) .3646(4) .7945(4) .040(2) Uani ? ? 1.00000 ? ?
H2a .3535 .3759 .4034 .041 Uiso ? ? 1.00000 ? ?
H2b .2855 .4445 .3576 .041 Uiso ? ? 1.00000 ? ?
H3a .3060 .3655 .1660 .049 Uiso ? ? 1.00000 ? ?
H3b .3729 .4409 .2071 .049 Uiso ? ? 1.00000 ? ?
H5a -.0954 .4447 .7554 .040 Uiso ? ? 1.00000 ? ?
H5b -.0968 .3787 .8801 .040 Uiso ? ? 1.00000 ? ?
H6a -.2108 .4401 .8324 .049 Uiso ? ? 1.00000 ? ?
H6b -.2064 .3632 .7133 .049 Uiso ? ? 1.00000 ? ?
H3 .0497 .2500 .2555 .057 Uiso ? ? 1.00000 ? ?
H3' -.0240 .2500 .3216 .057 Uiso ? ? 1.00000 ? ?
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Fe .301 .845 'Int Tables Vol IV Tables 2.2B and 2.3.1'
C .002 .002 'Int Tables Vol IV Tables 2.2B and 2.3.1'
H 0 0 'Int Tables Vol IV Tables 2.2B and 2.3.1'
N .004 .003 'Int Tables Vol IV Tables 2.2B and 2.3.1'
O .008 .006 'Int Tables Vol IV Tables 2.2B and 2.3.1'
F .014 .01 'Int Tables Vol IV Tables 2.2B and 2.3.1'
S .11 .124 'Int Tables Vol IV Tables 2.2B and 2.3.1'
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
F7a C7 F7c . . 109.0(5) ?
F7a C7 F7b . . 108.9(4) ?
F7a C7 S3 . . 109.5(4) ?
F7c C7 F7b . . 108.1(5) ?
F7c C7 S3 . . 111.8(4) ?
F7b C7 S3 . . 109.5(4) ?
O3a S3 O3b . . 118.6(2) ?
O3a S3 O3c . . 116.1(3) ?
O3a S3 C7 . . 104.02(17) ?
O3b S3 O3c . . 111.7(3) ?
O3b S3 C7 . . 104.0(2) ?
O3c S3 C7 . . 99.3(3) ?
O3 Fe S1 . . 99.38(9) y
O3 Fe S2 . . 104.42(9) y
S1 Fe S1 8 . 76.69(4) y
S1 Fe S2 . 8 156.19(5) y
S1 Fe S2 . . 98.46(4) y
S2 Fe S2 8 . 76.45(4) y
C1 S1 Fe . . 86.17(14) ?
C4 S2 Fe . . 86.70(14) ?
C1 N1 C2 . . 123.3(2) ?
C2 N1 C2 . 8 113.2(3) ?
C4 N2 C5 . . 123.3(2) ?
C5 N2 C5 8 . 113.4(3) ?
C3 O1 C3 . 8 111.3(3) ?
C6 O2 C6 8 . 110.1(3) ?
H3' O3 H3 . . 117.0 ?
H3' O3 Fe . . 119.1 ?
H3 O3 Fe . . 123.9 ?
N1 C1 S1 . . 124.86(13) ?
S1 C1 S1 8 . 110.3(3) ?
H2a C2 H2b . . 109.2 ?
H2a C2 N1 . . 109.7 ?
H2a C2 C3 . . 109.4 ?
H2b C2 N1 . . 109.9 ?
H2b C2 C3 . . 109.4 ?
N1 C2 C3 . . 109.1(3) ?
H3b C3 H3a . . 109.3 ?
H3b C3 O1 . . 109.3 ?
H3b C3 C2 . . 109.6 ?
H3a C3 O1 . . 109.3 ?
H3a C3 C2 . . 109.3 ?
O1 C3 C2 . . 110.0(3) ?
N2 C4 S2 . . 124.93(13) ?
S2 C4 S2 . 8 110.1(3) ?
H5a C5 H5b . . 109.4 ?
H5a C5 N2 . . 109.6 ?
H5a C5 C6 . . 109.7 ?
H5b C5 N2 . . 109.5 ?
H5b C5 C6 . . 109.4 ?
N2 C5 C6 . . 109.3(3) ?
H6a C6 H6b . . 109.3 ?
H6a C6 O2 . . 109.3 ?
H6a C6 C5 . . 109.1 ?
H6b C6 O2 . . 109.1 ?
H6b C6 C5 . . 109.0 ?
O2 C6 C5 . . 111.0(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
F7a C7 . . 1.322(7) ?
F7b C7 . . 1.326(7) ?
F7c C7 . . 1.325(5) ?
C7 S3 . . 1.775(5) ?
O3a S3 . . 1.400(3) ?
O3b S3 . . 1.441(4) ?
O3c S3 . . 1.457(5) ?
Fe O3 . . 2.013(4) y
Fe S1 . . 2.2849(11) y
Fe S2 . . 2.2870(11) y
S1 C1 . . 1.727(3) ?
S2 C4 . . 1.726(3) ?
N1 C1 . . 1.318(6) ?
N1 C2 . . 1.463(4) ?
N2 C4 . . 1.309(6) ?
N2 C5 . . 1.475(4) ?
O1 C3 . . 1.431(4) ?
O2 C6 . . 1.425(5) ?
O3 H3' . . .925 ?
O3 H3 . . .927 ?
C2 H2a . . .950 ?
C2 H2b . . .952 ?
C2 C3 . . 1.534(6) ?
C3 H3b . . .950 ?
C3 H3a . . .952 ?
C5 H5a . . .949 ?
C5 H5b . . .952 ?
C5 C6 . . 1.520(6) ?
C6 H6a . . .950 ?
C6 H6b . . .952 ?
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
_geom_hbond_publ_flag
O3 H3 O3b . 0.927 1.757 2.642(5) 158 y
O3 H3 O3b 8 0.927 1.757 2.642(5) 158 y
O3 H3' O1 3_455 0.925 1.732 2.654(5) 174 y
