#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/81/2238128.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_2238128
loop_
_publ_author_name
'Taş, Murat'
'Çamur, Seval'
'Topal, Sevim'
_publ_section_title
;
 Pentaaqua(dimethylformamide)cobalt(II) sulfate dimethylformamide
 monosolvate
;
_journal_coeditor_code           BQ2385
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m373
_journal_paper_doi               10.1107/S1600536813012841
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co (C3 H7 N O) (H2 O1)5] S O4, C3 H7 N O'
_chemical_formula_moiety         'C3 H17 Co N O6 2+, O4 S 2-, C3 H7 N O'
_chemical_formula_sum            'C6 H24 Co N2 O11 S'
_chemical_formula_weight         391.26
_chemical_name_systematic
;
Pentaaqua(dimethylformamide)cobalt(II) sulfate dimethylformamide monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.256(8)
_cell_length_b                   7.449(7)
_cell_length_c                   9.929(9)
_cell_measurement_reflns_used    108
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.8770
_cell_measurement_theta_min      4.3630
_cell_volume                     1646(2)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2011)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2011)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov et al., 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 16.0454
_diffrn_measured_fraction_theta_full 0.9888
_diffrn_measured_fraction_theta_max 0.9894
_diffrn_measurement_device_type
'Agilent SuperNova (Single source at offset, Eos)'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3903
_diffrn_reflns_theta_full        25.57
_diffrn_reflns_theta_max         25.57
_diffrn_reflns_theta_min         3.29
_exptl_absorpt_coefficient_mu    1.220
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SCALE3 in ABSPACK; Agilent, 2011)
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.189
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         1627
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0413
_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)+(0.0358P)²+1.4684P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                1407
_reflns_number_total             1627
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            bq2385.cif
_cod_data_source_block           I
_cod_database_code               2238128
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z+1/2'
4 '-x, y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z-1/2'
8 'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co1 0.14060(2) 0.2500 0.38601(6) 0.0369(2) Uani d S 1 2 . .
O O1 0.18765(17) 0.2500 0.2071(4) 0.0595(10) Uani d S 1 2 . .
H H1A 0.1918 0.3576 0.1787 0.089 Uiso d PR 0.50 1 . .
H H1B 0.1684 0.1889 0.1484 0.089 Uiso d PR 0.50 1 . .
O O2 0.19603(11) 0.0408(3) 0.4542(3) 0.0480(6) Uani d D 1 1 . .
O O4 0.09678(16) 0.2500 0.5671(4) 0.0554(9) Uani d S 1 2 . .
O O3 0.08065(10) 0.0530(3) 0.3135(3) 0.0491(6) Uani d D 1 1 . .
N N1 0.09188(18) 0.2500 0.7912(4) 0.0507(11) Uani d S 1 2 . .
C C1 0.1212(3) 0.2500 0.6752(6) 0.0581(14) Uani d S 1 2 . .
H H1 0.1630 0.2500 0.6774 0.070 Uiso calc SR 1 2 . .
C C3 0.1242(3) 0.2500 0.9139(6) 0.090(2) Uani d S 1 2 . .
H H3C 0.1223 0.1329 0.9538 0.135 Uiso calc PR 0.50 1 A -1
H H3D 0.1069 0.3363 0.9743 0.135 Uiso calc PR 0.50 1 A -1
H H3E 0.1654 0.2809 0.8968 0.135 Uiso calc PR 0.50 1 A -1
C C2 0.0295(2) 0.2500 0.7952(6) 0.0671(16) Uani d S 1 2 . .
H H2C 0.0154 0.1316 0.8164 0.101 Uiso calc PR 0.50 1 B -1
H H2D 0.0140 0.2859 0.7091 0.101 Uiso calc PR 0.50 1 B -1
H H2E 0.0160 0.3325 0.8630 0.101 Uiso calc PR 0.50 1 B -1
S S1 0.31484(5) 0.2500 0.66245(12) 0.0364(3) Uani d S 1 2 . .
O O8 0.37947(14) 0.2500 0.6875(4) 0.0512(9) Uani d S 1 2 . .
O O7 0.28365(16) 0.2500 0.7907(4) 0.0557(9) Uani d S 1 2 . .
N N2 0.40622(18) 0.2500 0.2342(4) 0.0489(10) Uani d S 1 2 . .
O O5 0.49626(15) 0.2500 0.3358(4) 0.0607(10) Uani d S 1 2 . .
C C6 0.4297(3) 0.2500 0.0993(5) 0.0689(17) Uani d S 1 2 . .
H H6A 0.4029 0.1851 0.0413 0.103 Uiso calc PR 0.50 1 C -1
H H6B 0.4685 0.1936 0.0987 0.103 Uiso calc PR 0.50 1 C -1
H H6C 0.4334 0.3713 0.0680 0.103 Uiso calc PR 0.50 1 C -1
C C4 0.4415(2) 0.2500 0.3370(6) 0.0546(13) Uani d S 1 2 . .
H H4 0.4232 0.2500 0.4212 0.066 Uiso calc SR 1 2 . .
C C5 0.3412(2) 0.2500 0.2504(7) 0.0722(18) Uani d S 1 2 . .
H H5A 0.3313 0.2272 0.3430 0.108 Uiso calc PR 0.50 1 D -1
H H5B 0.3239 0.1581 0.1948 0.108 Uiso calc PR 0.50 1 D -1
H H5C 0.3254 0.3647 0.2243 0.108 Uiso calc PR 0.50 1 D -1
O O6 0.29865(11) 0.4135(3) 0.5871(2) 0.0539(7) Uani d . 1 1 . .
H H3A 0.0516(12) 0.090(5) 0.266(3) 0.067(13) Uiso d D 1 1 . .
H H3B 0.0944(16) -0.044(4) 0.274(4) 0.067(13) Uiso d D 1 1 . .
H H2A 0.2308(11) 0.065(6) 0.492(4) 0.082(15) Uiso d D 1 1 . .
H H2B 0.2032(17) -0.055(6) 0.404(4) 0.071(14) Uiso d . 1 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'
Co Co 0.3494 0.9721 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Co1 O2 . . 88.81(11)
O1 Co1 O2 . 8_565 88.81(11)
O1 Co1 O3 . 8_565 91.57(12)
O1 Co1 O3 . . 91.57(12)
O2 Co1 O2 . 8_565 95.9(5)
O2 Co1 O3 8_565 . 176.13(10)
O2 Co1 O3 8_565 8_565 88.0(5)
O2 Co1 O3 . . 88.0(5)
O2 Co1 O3 . 8_565 176.13(10)
O4 Co1 O1 . . 177.94(15)
O4 Co1 O2 . . 89.81(11)
O4 Co1 O2 . 8_565 89.81(11)
O4 Co1 O3 . . 89.90(11)
O4 Co1 O3 . 8_565 89.91(11)
O3 Co1 O3 8_565 . 88.2(5)
Co1 O1 H1A . . 109.8
Co1 O1 H1B . . 109.5
H1A O1 H1B . . 109.1
Co1 O2 H2A . . 120(3)
Co1 O2 H2B . . 122(3)
H2A O2 H2B . . 104(4)
C1 O4 Co1 . . 124.7(4)
Co1 O3 H3A . . 116(3)
Co1 O3 H3B . . 120(2)
H3A O3 H3B . . 106(4)
C1 N1 C3 . . 119.9(5)
C1 N1 C2 . . 121.2(5)
C2 N1 C3 . . 119.0(5)
O4 C1 N1 . . 123.6(5)
O4 C1 H1 . . 118.2
N1 C1 H1 . . 118.2
N1 C3 H3C . . 109.5
N1 C3 H3D . . 109.5
N1 C3 H3E . . 109.5
N1 C2 H2C . . 109.5
N1 C2 H2D . . 109.5
N1 C2 H2E . . 109.5
O8 S1 O6 . . 109.10(17)
O8 S1 O6 . 8_565 109.10(17)
O7 S1 O8 . . 108.8(2)
O7 S1 O6 . . 109.19(18)
O7 S1 O6 . 8_565 109.19(18)
O6 S1 O6 8_565 . 111.4(5)
C6 N2 C5 . . 117.7(5)
C4 N2 C6 . . 121.1(5)
C4 N2 C5 . . 121.2(5)
N2 C6 H6A . . 109.5
N2 C6 H6B . . 109.5
N2 C6 H6C . . 109.5
N2 C4 H4 . . 116.5
O5 C4 N2 . . 127.0(5)
O5 C4 H4 . . 116.5
N2 C5 H5A . . 109.5
N2 C5 H5B . . 109.5
N2 C5 H5C . . 109.5
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
Co1 O1 . 2.062(4) y
Co1 O2 8_565 2.101(10) ?
Co1 O2 . 2.101(10) y
Co1 O4 . 2.046(4) y
Co1 O3 . 2.110(9) y
Co1 O3 8_565 2.110(9) ?
O1 H1A . 0.8552 ?
O1 H1B . 0.8552 ?
O2 H2A . 0.878(19) ?
O2 H2B . 0.89(4) ?
O4 C1 . 1.203(7) ?
O3 H3A . 0.850(18) ?
O3 H3B . 0.879(19) ?
N1 C1 . 1.324(7) ?
N1 C3 . 1.414(7) ?
N1 C2 . 1.389(6) ?
C1 H1 . 0.9300 ?
C3 H3C . 0.9600 ?
C3 H3D . 0.9600 ?
C3 H3E . 0.9600 ?
C2 H2C . 0.9600 ?
C2 H2D . 0.9600 ?
C2 H2E . 0.9600 ?
S1 O8 . 1.460(3) ?
S1 O7 . 1.450(4) ?
S1 O6 . 1.474(3) ?
S1 O6 8_565 1.474(3) ?
N2 C6 . 1.437(6) ?
N2 C4 . 1.288(7) ?
N2 C5 . 1.457(6) ?
O5 C4 . 1.219(6) ?
C6 H6A . 0.9600 ?
C6 H6B . 0.9600 ?
C6 H6C . 0.9600 ?
C4 H4 . 0.9300 ?
C5 H5A . 0.9600 ?
C5 H5B . 0.9600 ?
C5 H5C . 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
_geom_hbond_publ_flag
O1 H1A O6 2_564 0.86 1.95 2.792(4) 171.4 y
O1 H1B O6 7_655 0.86 2.26 2.792(4) 120.3 y
C2 H2D O4 . 0.96 2.34 2.715(7) 102.9 ?
O3 H3A O5 3_455 0.850(18) 1.99(2) 2.807(8) 162(4) y
O3 H3B O8 2_554 0.879(19) 1.85(2) 2.731(17) 178(4) y
O2 H2A O6 8_565 0.878(19) 1.79(2) 2.660(3) 171(4) y
O2 H2B O7 2_554 0.89(4) 1.86(4) 2.745(15) 177(4) y
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
Co1 O4 C1 N1 . 180.0
O2 Co1 O4 C1 8_565 -47.92(7)
O2 Co1 O4 C1 . 47.92(7)
O3 Co1 O4 C1 . 135.93(6)
O3 Co1 O4 C1 8_565 -135.93(6)
C3 N1 C1 O4 . 180.0
C2 N1 C1 O4 . 0.0000(10)
C6 N2 C4 O5 . 0.0
C5 N2 C4 O5 . 180.0
