#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:22:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179374 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/71/4327163.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4327163
loop_
_publ_author_name
'M. Jaya Prakash'
'Slavi C. Sevov'
_publ_section_title
;
 Hydrogen-Bonded Inclusion Compounds with Reversed Polarity: Anionic
 Metal-Complexes and Cationic Organic Linkers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12739
_journal_page_last               12746
_journal_paper_doi               10.1021/ic2018715
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C12 H14 Co N3 O11'
_chemical_formula_weight         435.19
_chemical_name_common            Coenox2-BPYE-H2O
_chemical_name_systematic
; 
 ? 
;
_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                63.1380(10)
_cell_angle_beta                 77.106(2)
_cell_angle_gamma                80.187(2)
_cell_formula_units_Z            2
_cell_length_a                   6.7369(6)
_cell_length_b                   11.7201(10)
_cell_length_c                   12.3229(11)
_cell_measurement_temperature    119(2)
_cell_volume                     843.39(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    Diomand
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      119(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11479
_diffrn_reflns_theta_full        26.32
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.084
_exptl_absorpt_correction_T_max  0.897
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Blessing, R.H. (1995) Acta Cryst. A51, 33-38'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.948
_refine_diff_density_min         -1.052
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0411P)²+2.1514P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.0996
_reflns_number_gt                3209
_reflns_number_total             3416
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic2018715_si_002_6.cif
_cod_data_source_block           Coenox2-BPYE-H2O
_cod_database_code               4327163
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.70992(5) 0.76472(3) 0.73648(3) 0.01062(11) Uani 1 1 d .
O5 O 0.7278(3) 0.59739(17) 0.74302(17) 0.0148(4) Uani 1 1 d .
O4 O 1.0007(3) 0.76803(17) 0.70063(16) 0.0148(4) Uani 1 1 d .
O1 O 0.7195(3) 0.83970(18) 0.56301(16) 0.0152(4) Uani 1 1 d .
O8 O 0.7166(3) 0.67915(17) 0.90823(16) 0.0135(4) Uani 1 1 d .
O3 O 1.2475(3) 0.8360(2) 0.53619(18) 0.0205(4) Uani 1 1 d .
O6 O 0.7386(3) 0.39229(18) 0.88051(19) 0.0210(4) Uani 1 1 d .
O7 O 0.7414(3) 0.47992(18) 1.05719(17) 0.0199(4) Uani 1 1 d .
O2 O 0.9515(3) 0.8957(2) 0.39038(17) 0.0216(4) Uani 1 1 d .
C10 C 0.7316(4) 0.5556(2) 0.9502(2) 0.0135(5) Uani 1 1 d .
C9 C 0.7333(4) 0.5075(2) 0.8521(2) 0.0142(5) Uani 1 1 d .
C7 C 0.9016(4) 0.8559(2) 0.5026(2) 0.0138(5) Uani 1 1 d .
C12 C 0.3310(4) 0.8724(3) 0.8070(3) 0.0181(5) Uani 1 1 d .
H12B H 0.3386 0.8421 0.8952 0.022 Uiso 1 1 calc R
H12A H 0.1864 0.8974 0.7958 0.022 Uiso 1 1 calc R
C8 C 1.0683(4) 0.8179(2) 0.5847(2) 0.0133(5) Uani 1 1 d .
C6 C 0.9168(5) 0.5395(3) 0.5022(3) 0.0222(6) Uani 1 1 d .
C4 C 0.5955(5) 0.6606(3) 0.4364(3) 0.0218(6) Uani 1 1 d .
H4A H 0.5879 0.6949 0.4939 0.026 Uiso 1 1 calc R
C3 C 0.7623(4) 0.5766(3) 0.4221(3) 0.0198(6) Uani 1 1 d .
C11 C 0.4598(4) 0.9845(3) 0.7275(3) 0.0206(6) Uani 1 1 d .
H11A H 0.4368 1.0225 0.6410 0.025 Uiso 1 1 calc R
H11B H 0.4252 1.0515 0.7581 0.025 Uiso 1 1 calc R
C5 C 0.4431(5) 0.6936(3) 0.3680(3) 0.0224(6) Uani 1 1 d .
H5A H 0.3293 0.7500 0.3786 0.027 Uiso 1 1 calc R
C2 C 0.7687(4) 0.5313(3) 0.3337(3) 0.0218(6) Uani 1 1 d .
H2A H 0.8808 0.4752 0.3204 0.026 Uiso 1 1 calc R
C1 C 0.6139(5) 0.5677(3) 0.2665(3) 0.0234(6) Uani 1 1 d .
H1A H 0.6191 0.5374 0.2062 0.028 Uiso 1 1 calc R
N3 N 0.4170(3) 0.7710(2) 0.7656(2) 0.0146(4) Uani 1 1 d .
N2 N 0.6761(4) 0.9320(2) 0.7358(2) 0.0157(5) Uani 1 1 d .
N1 N 0.4544(4) 0.6463(2) 0.2859(2) 0.0218(5) Uani 1 1 d .
O20 O 0.1038(7) 0.2368(4) 0.9518(4) 0.0927(15) Uani 1 1 d .
O21 O 0.0810(4) 0.8070(2) 0.2096(2) 0.0385(6) Uani 1 1 d .
O22 O 0.3069(6) 1.0087(3) 0.0545(3) 0.0645(9) Uani 1 1 d .
H1B H 0.356(6) 0.668(4) 0.244(4) 0.038(11) Uiso 1 1 d .
H6A H 0.890(5) 0.569(3) 0.569(3) 0.026(9) Uiso 1 1 d .
H3B H 0.371(5) 0.701(3) 0.819(3) 0.020(8) Uiso 1 1 d .
H2C H 0.700(5) 0.928(3) 0.800(3) 0.017(8) Uiso 1 1 d .
H3A H 0.381(5) 0.790(3) 0.694(3) 0.018(8) Uiso 1 1 d .
H2B H 0.752(6) 0.982(4) 0.678(4) 0.030(10) Uiso 1 1 d .
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
_geom_angle_site_symmetry_1
O8 Co1 O1 175.28(8) .
O8 Co1 O5 85.99(8) .
O1 Co1 O5 90.34(8) .
O8 Co1 O4 90.99(8) .
O1 Co1 O4 86.14(8) .
O5 Co1 O4 91.77(8) .
O8 Co1 N3 91.35(9) .
O1 Co1 N3 91.65(9) .
O5 Co1 N3 90.51(9) .
O4 Co1 N3 176.84(9) .
O8 Co1 N2 92.65(9) .
O1 Co1 N2 91.17(10) .
O5 Co1 N2 176.62(9) .
O4 Co1 N2 91.34(9) .
N3 Co1 N2 86.43(10) .
C9 O5 Co1 112.84(16) .
C8 O4 Co1 112.42(16) .
C7 O1 Co1 112.94(16) .
C10 O8 Co1 112.99(16) .
O7 C10 O8 125.2(2) .
O7 C10 C9 120.8(2) .
O8 C10 C9 114.0(2) .
O6 C9 O5 125.1(2) .
O6 C9 C10 120.8(2) .
O5 C9 C10 114.1(2) .
O2 C7 O1 126.2(2) .
O2 C7 C8 119.7(2) .
O1 C7 C8 114.0(2) .
N3 C12 C11 105.7(2) .
O3 C8 O4 126.0(2) .
O3 C8 C7 119.7(2) .
O4 C8 C7 114.3(2) .
C6 C6 C3 124.1(4) 2_766
C5 C4 C3 120.4(3) .
C4 C3 C2 117.5(3) .
C4 C3 C6 118.1(3) .
C2 C3 C6 124.3(3) .
N2 C11 C12 106.1(2) .
N1 C5 C4 119.9(3) .
C1 C2 C3 120.1(3) .
N1 C1 C2 120.0(3) .
C12 N3 Co1 109.40(17) .
C11 N2 Co1 109.15(17) .
C5 N1 C1 122.0(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O8 1.8964(18) .
Co1 O1 1.8990(18) .
Co1 O5 1.9100(18) .
Co1 O4 1.9125(18) .
Co1 N3 1.920(2) .
Co1 N2 1.931(2) .
O5 C9 1.284(3) .
O4 C8 1.279(3) .
O1 C7 1.281(3) .
O8 C10 1.293(3) .
O3 C8 1.229(3) .
O6 C9 1.229(3) .
O7 C10 1.221(3) .
O2 C7 1.227(3) .
C10 C9 1.545(4) .
C7 C8 1.553(4) .
C12 N3 1.480(3) .
C12 C11 1.511(4) .
C6 C6 1.334(6) 2_766
C6 C3 1.471(4) .
C4 C5 1.368(4) .
C4 C3 1.398(4) .
C3 C2 1.401(4) .
C11 N2 1.489(3) .
C5 N1 1.339(4) .
C2 C1 1.367(4) .
C1 N1 1.344(4) .
