#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:45:49 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180517 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/86/7218604.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_7218604
loop_
_publ_author_name
'Li, Quan-Quan'
'Kang, Yi-Fan'
'Ren, Chun-Yan'
'Yang, Guo-Ping'
'Liu, Qing Liu, Ping'
'Wang, Yao-Yu'
_publ_section_title
;
 Reaction-controlled assemblies and structural diversities of seven
 Co(ii)/Cu(ii) complexes based on a bipyridine-dicarboxylate N-oxide
 ligand
;
_journal_issue                   4
_journal_name_full               CrystEngComm
_journal_page_first              775
_journal_paper_doi               10.1039/C4CE02008A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C14 H11 Co N3 O8'
_chemical_formula_weight         408.17
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.971(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.462(2)
_cell_length_b                   15.486(3)
_cell_length_c                   7.4899(12)
_cell_measurement_reflns_used    533
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.305
_cell_measurement_theta_min      2.630
_cell_volume                     1665.0(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0615
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4251
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.080
_exptl_absorpt_correction_T_max  0.7713
_exptl_absorpt_correction_T_min  0.7346
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         1538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0642
_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)+(0.1026P)²+2.8144P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1755
_refine_ls_wR_factor_ref         0.1940
_reflns_number_gt                1105
_reflns_number_total             1538
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce02008a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7218604--7218608.cif.'
_cod_original_sg_symbol_H-M      'C2/m  '
_cod_database_code               7218604
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.0000 0.5000 0.5000 0.0286(4) Uani 1 4 d S
Co2 Co 0.0000 0.0000 0.0000 0.0394(5) Uani 1 4 d S
O1 O -0.0678(3) 0.3501(3) 0.1870(7) 0.0641(15) Uani 1 1 d .
O2 O 0.0566(3) 0.4055(3) 0.3484(7) 0.0560(13) Uani 1 1 d .
O3 O 0.0740(3) 0.0977(2) -0.1085(5) 0.0419(10) Uani 1 1 d .
O4 O 0.1292(3) 0.5000 0.6724(7) 0.0409(14) Uani 1 2 d S
N1 N 0.0820(6) 0.0000 0.2538(10) 0.052(2) Uani 1 2 d S
N2 N 0.1051(3) 0.1569(3) 0.0140(6) 0.0346(11) Uani 1 1 d .
C1 C 0.0159(4) 0.3509(4) 0.2461(8) 0.0403(14) Uani 1 1 d .
C2 C 0.0787(4) 0.2801(3) 0.1861(7) 0.0332(12) Uani 1 1 d .
C3 C 0.1692(4) 0.2736(4) 0.2697(8) 0.0435(15) Uani 1 1 d .
H3 H 0.1907 0.3125 0.3599 0.052 Uiso 1 1 calc R
C4 C 0.2273(4) 0.2103(4) 0.2204(8) 0.0454(15) Uani 1 1 d .
H4 H 0.2887 0.2073 0.2736 0.054 Uiso 1 1 calc R
C5 C 0.1937(4) 0.1512(4) 0.0916(8) 0.0451(15) Uani 1 1 d .
H5 H 0.2322 0.1074 0.0583 0.054 Uiso 1 1 calc R
C6 C 0.0470(3) 0.2214(3) 0.0540(7) 0.0315(12) Uani 1 1 d .
C7 C 0.1253(9) 0.0000 0.3881(19) 0.076(3) Uani 1 2 d S
C8 C 0.1888(12) 0.0000 0.5661(16) 0.123(6) Uani 1 2 d S
H8A H 0.2503 0.0178 0.5458 0.148 Uiso 0.50 1 d PR
H8B H 0.1915 -0.0571 0.6163 0.148 Uiso 0.50 1 d PR
H8C H 0.1648 0.0393 0.6482 0.148 Uiso 0.50 1 d PR
O5 O 0.3335(6) 0.0000 0.9157(13) 0.097(3) Uani 1 2 d S
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'
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
_geom_angle_site_symmetry_3
O2 Co1 O2 180 . 5_566
O2 Co1 O2 89.4(3) . 6_565
O2 Co1 O2 90.6(3) 5_566 6_565
O2 Co1 O2 90.6(3) . 2_556
O2 Co1 O2 89.4(3) 5_566 2_556
O2 Co1 O2 180 6_565 2_556
O2 Co1 O4 87.52(16) . .
O2 Co1 O4 92.48(16) 5_566 .
O2 Co1 O4 87.52(16) 6_565 .
O2 Co1 O4 92.48(16) 2_556 .
O2 Co1 O4 92.48(16) . 5_566
O2 Co1 O4 87.52(16) 5_566 5_566
O2 Co1 O4 92.48(15) 6_565 5_566
O2 Co1 O4 87.52(16) 2_556 5_566
O4 Co1 O4 180 . 5_566
O3 Co2 O3 86.4(2) 5 6
O3 Co2 O3 93.6(2) 5 2
O3 Co2 O3 180 6 2
O3 Co2 O3 180 5 .
O3 Co2 O3 93.6(2) 6 .
O3 Co2 O3 86.4(2) 2 .
O3 Co2 N1 84.69(18) 5 .
O3 Co2 N1 95.31(18) 6 .
O3 Co2 N1 84.69(18) 2 .
O3 Co2 N1 95.31(18) . .
O3 Co2 N1 95.31(18) 5 5
O3 Co2 N1 84.69(18) 6 5
O3 Co2 N1 95.31(18) 2 5
O3 Co2 N1 84.69(18) . 5
N1 Co2 N1 180 . 5
C1 O2 Co1 128.9(4) . .
N2 O3 Co2 112.2(3) . .
C7 N1 Co2 180 . .
O3 N2 C5 118.4(5) . .
O3 N2 C6 119.3(4) . .
C5 N2 C6 122.2(5) . .
O1 C1 O2 126.7(5) . .
O1 C1 C2 118.6(5) . .
O2 C1 C2 114.6(5) . .
C6 C2 C3 119.3(5) . .
C6 C2 C1 121.8(5) . .
C3 C2 C1 118.9(5) . .
C4 C3 C2 120.5(6) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C3 C4 C5 119.3(6) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
N2 C5 C4 119.8(5) . .
N2 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
N2 C6 C2 118.8(5) . .
N2 C6 C6 115.2(4) . 2
C2 C6 C6 126.0(4) . 2
N1 C7 C8 177.1(14) . .
C7 C8 H8A 109.5 . .
C7 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C7 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 2.080(4) .
Co1 O2 2.080(4) 5_566
Co1 O2 2.080(4) 6_565
Co1 O2 2.080(4) 2_556
Co1 O4 2.138(5) .
Co1 O4 2.138(5) 5_566
Co2 O3 2.075(4) 5
Co2 O3 2.075(4) 6
Co2 O3 2.075(4) 2
Co2 O3 2.075(4) .
Co2 N1 2.115(8) .
Co2 N1 2.115(8) 5
O1 C1 1.237(7) .
O2 C1 1.241(7) .
O3 N2 1.336(6) .
N1 C7 1.119(14) .
N2 C5 1.345(7) .
N2 C6 1.361(7) .
C1 C2 1.525(7) .
C2 C6 1.381(7) .
C2 C3 1.384(7) .
C3 C4 1.371(8) .
C3 H3 0.9300 .
C4 C5 1.375(8) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 C6 1.496(10) 2
C7 C8 1.524(19) .
C8 H8A 0.9600 .
C8 H8B 0.9599 .
C8 H8C 0.9601 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O2 Co1 O2 C1 -115.7(5) 6_565 .
O2 Co1 O2 C1 64.3(5) 2_556 .
O4 Co1 O2 C1 156.8(6) . .
O4 Co1 O2 C1 -23.2(6) 5_566 .
O3 Co2 O3 N2 -130.4(3) 6 .
O3 Co2 O3 N2 49.6(3) 2 .
N1 Co2 O3 N2 -34.8(4) . .
N1 Co2 O3 N2 145.2(4) 5 .
Co2 O3 N2 C5 98.0(5) . .
Co2 O3 N2 C6 -83.1(5) . .
Co1 O2 C1 O1 13.7(10) . .
Co1 O2 C1 C2 -168.2(4) . .
O1 C1 C2 C6 7.1(9) . .
O2 C1 C2 C6 -171.1(5) . .
O1 C1 C2 C3 -171.3(6) . .
O2 C1 C2 C3 10.4(8) . .
C6 C2 C3 C4 0.9(9) . .
C1 C2 C3 C4 179.3(6) . .
C2 C3 C4 C5 -2.4(9) . .
O3 N2 C5 C4 -178.9(5) . .
C6 N2 C5 C4 2.2(8) . .
C3 C4 C5 N2 0.9(9) . .
O3 N2 C6 C2 177.4(4) . .
C5 N2 C6 C2 -3.7(8) . .
O3 N2 C6 C6 -2.9(7) . 2
C5 N2 C6 C6 175.9(5) . 2
C3 C2 C6 N2 2.1(8) . .
C1 C2 C6 N2 -176.3(5) . .
C3 C2 C6 C6 -177.5(5) . 2
C1 C2 C6 C6 4.1(9) . 2
