#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/55/2225561.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_2225561
loop_
_publ_author_name
'Sarkar, Bipasa'
'Roy, Abhijit'
'Ng, Seik Weng'
'Tiekink, Edward R. T.'
_publ_section_title
;
 Bis(3,5-dinitrobenzoato-κO¹)tetramethanolcobalt(II)
;
_journal_coeditor_code           HB5347
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m365
_journal_paper_doi               10.1107/S1600536810007580
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Co (C7 H3 N2 O6)2 (C H4 O)4]'
_chemical_formula_moiety         'C18 H22 Co N4 O16'
_chemical_formula_sum            'C18 H22 Co N4 O16'
_chemical_formula_weight         609.33
_chemical_name_systematic
;
Bis(3,5-dinitrobenzoato-κO¹)tetramethanolcobalt(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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.411(2)
_cell_angle_beta                 100.407(2)
_cell_angle_gamma                102.214(2)
_cell_formula_units_Z            1
_cell_length_a                   6.4068(8)
_cell_length_b                   8.7660(11)
_cell_length_c                   12.1603(16)
_cell_measurement_reflns_used    1592
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.8
_cell_measurement_theta_min      2.4
_cell_volume                     655.78(14)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX diffractometer'
_diffrn_measurement_method       'ω scans'
_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  0.028
_diffrn_reflns_av_sigmaI/netI    0.044
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6372
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         1.7
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             313
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.38
_refine_diff_density_min         -0.30
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2999
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.060
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0522P)²+0.1427P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.100
_refine_ls_wR_factor_ref         0.110
_reflns_number_gt                2388
_reflns_number_total             2999
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb5347.cif
_cod_data_source_block           I
_cod_original_cell_volume        655.77(14)
_cod_database_code               2225561
_cod_database_fobs_code          2225561
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
Co Co 0.5000 0.5000 0.5000 0.03530(16) Uani d S 1 . .
O O1 0.6891(3) 0.3924(2) 0.61732(14) 0.0514(5) Uani d . 1 . .
O O2 0.8795(3) 0.2811(2) 0.51696(14) 0.0471(4) Uani d . 1 . .
O O3 1.4087(5) 0.0083(4) 0.7142(2) 0.1213(12) Uani d . 1 . .
O O4 1.4957(5) 0.0210(4) 0.8875(2) 0.1234(12) Uani d . 1 . .
O O5 1.0327(5) 0.2304(4) 1.1038(2) 0.1159(11) Uani d . 1 . .
O O6 0.8093(6) 0.3608(4) 1.0193(2) 0.1090(10) Uani d . 1 . .
O O7 0.3342(3) 0.5533(2) 0.62522(14) 0.0458(4) Uani d D 1 . .
H H7O 0.255(4) 0.614(3) 0.595(2) 0.075(11) Uiso d D 1 . .
O O8 0.2673(3) 0.2953(2) 0.46261(18) 0.0550(5) Uani d D 1 . .
H H8O 0.145(3) 0.291(4) 0.481(3) 0.075(10) Uiso d D 1 . .
N N1 1.3845(5) 0.0471(3) 0.8033(2) 0.0710(8) Uani d . 1 . .
N N2 0.9450(5) 0.2836(4) 1.0197(2) 0.0775(8) Uani d . 1 . .
C C1 0.8312(4) 0.3181(3) 0.60687(19) 0.0379(5) Uani d . 1 . .
C C2 0.9496(4) 0.2659(3) 0.7142(2) 0.0383(5) Uani d . 1 . .
C C3 1.1103(4) 0.1830(3) 0.7114(2) 0.0420(6) Uani d . 1 . .
H H3 1.1468 0.1592 0.6436 0.050 Uiso calc R 1 . .
C C4 1.2149(4) 0.1366(3) 0.8100(2) 0.0498(6) Uani d . 1 . .
C C5 1.1687(5) 0.1679(3) 0.9125(2) 0.0547(7) Uani d . 1 . .
H H5 1.2420 0.1356 0.9783 0.066 Uiso calc R 1 . .
C C6 1.0075(5) 0.2500(3) 0.9125(2) 0.0525(7) Uani d . 1 . .
C C7 0.8985(4) 0.2998(3) 0.8158(2) 0.0468(6) Uani d . 1 . .
H H7 0.7914 0.3558 0.8191 0.056 Uiso calc R 1 . .
C C8 0.4162(5) 0.5914(4) 0.7407(2) 0.0604(8) Uani d . 1 . .
H H8A 0.3034 0.6156 0.7755 0.091 Uiso calc R 1 . .
H H8B 0.5356 0.6803 0.7491 0.091 Uiso calc R 1 . .
H H8C 0.4652 0.5041 0.7755 0.091 Uiso calc R 1 . .
C C9 0.2797(6) 0.1460(3) 0.4244(3) 0.0787(11) Uani d . 1 . .
H H9A 0.2018 0.1255 0.3487 0.118 Uiso calc R 1 . .
H H9B 0.2166 0.0686 0.4712 0.118 Uiso calc R 1 . .
H H9C 0.4292 0.1422 0.4271 0.118 Uiso calc R 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'
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
_geom_angle_publ_flag
O8 Co O1 . . 91.36(8) ?
O8 Co O1 2_666 . 88.64(8) ?
O8 Co O1 . 2_666 88.64(8) ?
O8 Co O1 2_666 2_666 91.36(8) ?
O8 Co O7 . . 88.14(7) ?
O8 Co O7 2_666 . 91.86(7) ?
O1 Co O7 . . 89.22(7) ?
O1 Co O7 2_666 . 90.78(7) ?
O8 Co O7 . 2_666 91.86(7) ?
O8 Co O7 2_666 2_666 88.14(7) ?
O1 Co O7 . 2_666 90.78(7) ?
O1 Co O7 2_666 2_666 89.22(7) ?
O1 Co O1 . 2_666 180.0 n
O7 Co O7 . 2_666 180.0 n
O8 Co O8 . 2_666 180.0 n
C1 O1 Co . . 130.70(16) ?
C8 O7 Co . . 128.82(16) ?
C8 O7 H7O . . 113(2) ?
Co O7 H7O . . 105(2) ?
C9 O8 Co . . 131.57(18) ?
C9 O8 H8O . . 110(2) ?
Co O8 H8O . . 118(2) ?
O3 N1 O4 . . 122.3(3) ?
O3 N1 C4 . . 118.6(3) ?
O4 N1 C4 . . 119.1(3) ?
O6 N2 O5 . . 123.7(3) ?
O6 N2 C6 . . 118.5(3) ?
O5 N2 C6 . . 117.8(3) ?
O2 C1 O1 . . 126.1(2) ?
O2 C1 C2 . . 118.0(2) ?
O1 C1 C2 . . 115.9(2) ?
C7 C2 C3 . . 119.3(2) ?
C7 C2 C1 . . 120.5(2) ?
C3 C2 C1 . . 120.2(2) ?
C4 C3 C2 . . 119.1(2) ?
C4 C3 H3 . . 120.5 ?
C2 C3 H3 . . 120.5 ?
C5 C4 C3 . . 123.3(2) ?
C5 C4 N1 . . 119.3(2) ?
C3 C4 N1 . . 117.4(2) ?
C4 C5 C6 . . 116.3(2) ?
C4 C5 H5 . . 121.9 ?
C6 C5 H5 . . 121.9 ?
C5 C6 C7 . . 122.6(2) ?
C5 C6 N2 . . 119.1(3) ?
C7 C6 N2 . . 118.3(3) ?
C6 C7 C2 . . 119.4(2) ?
C6 C7 H7 . . 120.3 ?
C2 C7 H7 . . 120.3 ?
O7 C8 H8A . . 109.5 ?
O7 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
O7 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
O8 C9 H9A . . 109.5 ?
O8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
O8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 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
Co O8 . 2.0645(18) y
Co O8 2_666 2.0645(18) ?
Co O1 . 2.0666(17) y
Co O1 2_666 2.0666(16) ?
Co O7 . 2.1094(16) y
Co O7 2_666 2.1094(16) ?
O1 C1 . 1.250(3) ?
O2 C1 . 1.247(3) ?
O3 N1 . 1.179(4) ?
O4 N1 . 1.190(3) ?
O5 N2 . 1.220(4) ?
O6 N2 . 1.209(4) ?
O7 C8 . 1.418(3) ?
O7 H7O . 0.85(3) ?
O8 C9 . 1.408(3) ?
O8 H8O . 0.85(3) ?
N1 C4 . 1.482(3) ?
N2 C6 . 1.476(4) ?
C1 C2 . 1.511(3) ?
C2 C7 . 1.380(3) ?
C2 C3 . 1.385(3) ?
C3 C4 . 1.373(3) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.371(4) ?
C5 C6 . 1.378(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.379(4) ?
C7 H7 . 0.9300 ?
C8 H8A . 0.9600 ?
C8 H8B . 0.9600 ?
C8 H8C . 0.9600 ?
C9 H9A . 0.9600 ?
C9 H9B . 0.9600 ?
C9 H9C . 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
O7 H7o O2 2_666 0.85(3) 1.840(15) 2.645(2) 158(3)
O8 H8o O2 1_455 0.85(3) 1.817(10) 2.662(2) 179(3)
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
O8 Co O1 C1 . . . . 87.5(2) ?
O8 Co O1 C1 2_666 . . . -92.5(2) ?
O7 Co O1 C1 . . . . 175.6(2) ?
O7 Co O1 C1 2_666 . . . -4.4(2) ?
O8 Co O7 C8 . . . . 125.9(2) ?
O8 Co O7 C8 2_666 . . . -54.1(2) ?
O1 Co O7 C8 . . . . 34.5(2) ?
O1 Co O7 C8 2_666 . . . -145.5(2) ?
O1 Co O8 C9 . . . . -58.0(3) ?
O1 Co O8 C9 2_666 . . . 122.0(3) ?
O7 Co O8 C9 . . . . -147.1(3) ?
O7 Co O8 C9 2_666 . . . 32.9(3) ?
Co O1 C1 O2 . . . . -6.2(4) ?
Co O1 C1 C2 . . . . 175.42(15) ?
O2 C1 C2 C7 . . . . -178.2(2) ?
O1 C1 C2 C7 . . . . 0.3(4) ?
O2 C1 C2 C3 . . . . 1.6(4) ?
O1 C1 C2 C3 . . . . -179.9(2) ?
C7 C2 C3 C4 . . . . 0.0(4) ?
C1 C2 C3 C4 . . . . -179.8(2) ?
C2 C3 C4 C5 . . . . 0.0(4) ?
C2 C3 C4 N1 . . . . 179.5(2) ?
O3 N1 C4 C5 . . . . 173.0(3) ?
O4 N1 C4 C5 . . . . -9.2(5) ?
O3 N1 C4 C3 . . . . -6.5(5) ?
O4 N1 C4 C3 . . . . 171.2(3) ?
C3 C4 C5 C6 . . . . 0.2(4) ?
N1 C4 C5 C6 . . . . -179.3(3) ?
C4 C5 C6 C7 . . . . -0.5(4) ?
C4 C5 C6 N2 . . . . 178.2(3) ?
O6 N2 C6 C5 . . . . 177.2(3) ?
O5 N2 C6 C5 . . . . -3.4(5) ?
O6 N2 C6 C7 . . . . -4.0(5) ?
O5 N2 C6 C7 . . . . 175.4(3) ?
C5 C6 C7 C2 . . . . 0.6(4) ?
N2 C6 C7 C2 . . . . -178.1(3) ?
C3 C2 C7 C6 . . . . -0.3(4) ?
C1 C2 C7 C6 . . . . 179.5(2) ?
