#------------------------------------------------------------------------------
#$Date: 2016-02-21 11:56:54 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176809 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/04/2240473.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_2240473
loop_
_publ_author_name
'Held, Peter'
_publ_section_title
;
 Crystal structure of bis(dimethylammonium) hexaaquacobalt(II)
 bis(sulfate) dihydrate
;
_journal_coeditor_code           FK2085
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m77
_journal_page_last               m78
_journal_paper_doi               10.1107/S2056989015003400
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C2 H8 N)2 [Co (H2 O)6] (S O4)2, 2H2 O'
_chemical_formula_moiety         'Co H12 O6, 2(O4 S), 2(C2 H8 N), 2(H2 O)'
_chemical_formula_sum            'C4 H32 Co N2 O16 S2'
_chemical_formula_weight         487.37
_chemical_name_common
;
Bis(dimethylammonium) hexaaquacobalt(II) bis(sulfate) dihydrate
;
_chemical_name_systematic
;
Bis(dimethylammonium) hexaaquacobalt(II) bis(sulfate) dihydrate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.975(5)
_cell_length_b                   13.268(5)
_cell_length_c                   16.528(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.79
_cell_measurement_theta_min      12.02
_cell_volume                     1968.2(15)
_computing_cell_refinement
;
CAD-4 EXPRESS (Enraf--Nonius, 1989)
;
_computing_data_collection
;
CAD-4 EXPRESS (Enraf--Nonius, 1989)
;
_computing_data_reduction
;
MolEN (Fair, 1990)
;
_computing_molecular_graphics
;
ATOMS (Dowty, 2011)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR97 (Altomare et al.,  1999)
;
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       ω/2θ
_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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3383
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        1.50
_diffrn_standards_interval_count 100
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.9996
_exptl_absorpt_correction_T_min  0.9026
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al.,  1968)
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.368
_refine_ls_extinction_coef       0.0022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         1733
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0393
_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)+(0.0529P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.1109
_reflns_number_gt                936
_reflns_number_total             1733
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            fk2085sup1.cf
_cod_data_source_block           I
_cod_database_code               2240473
_cod_database_fobs_code          2240473
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
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_symmetry_multiplicity
Co Co 0.0000 0.5000 0.5000 0.0278(3) Uani d S 1 2
S S1 0.44510(13) 0.65726(9) 0.59555(8) 0.0319(3) Uani d . 1 1
O O1 0.3702(4) 0.6999(2) 0.5243(2) 0.0466(10) Uani d . 1 1
O O2 0.3355(4) 0.6107(3) 0.6497(2) 0.0419(9) Uani d . 1 1
O O3 0.5255(5) 0.7366(3) 0.6378(2) 0.0634(12) Uani d . 1 1
O O4 0.5493(5) 0.5793(3) 0.5696(3) 0.0791(15) Uani d . 1 1
O O5 -0.0505(5) 0.4446(3) 0.3854(2) 0.0422(10) Uani d . 1 1
H H51 -0.136(7) 0.422(4) 0.380(3) 0.040(18) Uiso d . 1 1
H H52 0.010(8) 0.403(5) 0.365(5) 0.11(3) Uiso d . 1 1
O O6 0.1413(5) 0.6068(3) 0.4439(3) 0.0391(10) Uani d . 1 1
H H61 0.103(8) 0.653(5) 0.415(4) 0.09(3) Uiso d . 1 1
H H62 0.198(6) 0.620(4) 0.470(3) 0.03(2) Uiso d . 1 1
O O7 0.1808(5) 0.4036(3) 0.5066(3) 0.0444(10) Uani d . 1 1
H H71 0.251(7) 0.412(4) 0.484(3) 0.037(19) Uiso d . 1 1
H H72 0.172(5) 0.350(3) 0.512(3) 0.021(16) Uiso d . 1 1
O O8 0.1675(5) 0.3224(4) 0.3135(3) 0.0558(13) Uani d . 1 1
H H81 0.245(7) 0.326(5) 0.322(4) 0.06(2) Uiso d . 1 1
H H82 0.174(8) 0.348(5) 0.268(4) 0.09(3) Uiso d . 1 1
N N3 0.0327(6) 0.1120(3) 0.3563(3) 0.0567(14) Uani d . 1 1
H H3A 0.1016 0.1541 0.3769 0.068 Uiso calc R 1 1
H H3B 0.0187 0.0622 0.3925 0.068 Uiso calc R 1 1
C C1 0.0909(10) 0.0689(5) 0.2833(4) 0.094(3) Uani d . 1 1
H H1A 0.1825 0.0344 0.2950 0.141 Uiso calc R 1 1
H H1B 0.1092 0.1214 0.2446 0.141 Uiso calc R 1 1
H H1C 0.0201 0.0219 0.2615 0.141 Uiso calc R 1 1
C C2 -0.1060(7) 0.1669(5) 0.3473(4) 0.074(2) Uani d . 1 1
H H2A -0.1450 0.1833 0.3998 0.111 Uiso calc R 1 1
H H2B -0.1767 0.1260 0.3187 0.111 Uiso calc R 1 1
H H2C -0.0883 0.2279 0.3175 0.111 Uiso calc R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
Co Co 0.3494 0.9721 '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
O7 Co O7 5_566 . 180.0(3)
O7 Co O5 5_566 5_566 90.04(18)
O7 Co O5 . 5_566 89.96(18)
O7 Co O5 5_566 . 89.96(18)
O7 Co O5 . . 90.04(18)
O5 Co O5 5_566 . 180.0000(10)
O7 Co O6 5_566 . 91.87(19)
O7 Co O6 . . 88.13(19)
O5 Co O6 5_566 . 91.80(18)
O5 Co O6 . . 88.20(18)
O7 Co O6 5_566 5_566 88.13(19)
O7 Co O6 . 5_566 91.87(19)
O5 Co O6 5_566 5_566 88.20(18)
O5 Co O6 . 5_566 91.80(18)
O6 Co O6 . 5_566 180.0
O3 S1 O4 . . 109.6(3)
O3 S1 O2 . . 110.1(2)
O4 S1 O2 . . 108.1(2)
O3 S1 O1 . . 109.5(2)
O4 S1 O1 . . 109.3(3)
O2 S1 O1 . . 110.2(2)
Co O5 H51 . . 116(4)
Co O5 H52 . . 117(5)
H51 O5 H52 . . 108(6)
Co O6 H61 . . 119(5)
Co O6 H62 . . 109(4)
H61 O6 H62 . . 119(6)
Co O7 H71 . . 123(4)
Co O7 H72 . . 122(4)
H71 O7 H72 . . 109(6)
H81 O8 H82 . . 95(7)
C1 N3 C2 . . 115.3(5)
C1 N3 H3A . . 108.5
C2 N3 H3A . . 108.5
C1 N3 H3B . . 108.5
C2 N3 H3B . . 108.5
H3A N3 H3B . . 107.5
N3 C1 H1A . . 109.5
N3 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
N3 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
N3 C2 H2A . . 109.5
N3 C2 H2B . . 109.5
H2A C2 H2B . . 109.5
N3 C2 H2C . . 109.5
H2A C2 H2C . . 109.5
H2B C2 H2C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co O7 5_566 2.069(4)
Co O7 . 2.069(4)
Co O5 5_566 2.081(4)
Co O5 . 2.081(4)
Co O6 . 2.116(4)
Co O6 5_566 2.116(4)
S1 O3 . 1.454(4)
S1 O4 . 1.459(4)
S1 O2 . 1.467(3)
S1 O1 . 1.470(3)
O5 H51 . 0.82(6)
O5 H52 . 0.84(7)
O6 H61 . 0.85(7)
O6 H62 . 0.69(5)
O7 H71 . 0.74(6)
O7 H72 . 0.72(4)
O8 H81 . 0.71(6)
O8 H82 . 0.83(6)
N3 C1 . 1.434(7)
N3 C2 . 1.450(7)
N3 H3A . 0.9000
N3 H3B . 0.9000
C1 H1A . 0.9600
C1 H1B . 0.9600
C1 H1C . 0.9600
C2 H2A . 0.9600
C2 H2B . 0.9600
C2 H2C . 0.9600
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
O5 H51 O2 5_566 0.82(6) 1.91(6) 2.724(6) 169(5)
O5 H52 O8 . 0.84(7) 1.97(8) 2.806(7) 171(7)
O6 H61 O3 3_466 0.85(7) 1.85(7) 2.687(6) 173(6)
O6 H62 O1 . 0.69(5) 2.08(5) 2.740(6) 161(6)
O7 H71 O4 5_666 0.74(6) 2.01(6) 2.740(6) 173(6)
O7 H72 O1 7_655 0.72(4) 2.04(4) 2.756(6) 176(5)
O8 H81 O3 5_666 0.71(6) 2.32(6) 2.975(7) 154(7)
O8 H82 O2 2_564 0.83(6) 2.02(6) 2.849(6) 169(7)
N3 H3A O6 7_655 0.90 2.63 3.265(6) 127.8
N3 H3B O4 3_456 0.90 2.00 2.823(6) 151.5
