#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:12:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179317 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/14/4321477.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_4321477
loop_
_publ_author_name
'Yu-Bin Dong'
'Mark D. Smith'
'Hans-Conrad zur Loye'
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina  29208
USA
;
_publ_contact_author_email       ' zurloye@sc.edu'
_publ_contact_author_name        'Hans-Conrad zur Loye'
_publ_section_title
;
 New Inorganic/Organic Coordination Polymers Generated from Bidentate
 Schiff-Base Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4927
_journal_page_last               4935
_journal_paper_doi               10.1021/ic0006504
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C18 H17 Co N8 O7'
_chemical_formula_weight         516.33
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           68
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2a 2ac'
_symmetry_space_group_name_H-M   'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and manual editing'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.031(4)
_cell_length_b                   33.627(7)
_cell_length_c                   14.299(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     9151(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan (MSC, 1992-1997)'
_computing_publication_material  'SHELXTL (BRUKER) '
_computing_structure_refinement  'SHELXTL (BRUKER) '
_computing_structure_solution    'SHELXTL (BRUKER) '
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3373
_diffrn_reflns_theta_full        23.48
_diffrn_reflns_theta_max         23.48
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        -0.2
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.806
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.478
_exptl_absorpt_correction_type   difabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4192
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.065
_refine_ls_extinction_coef       0.00021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3373
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0474P)²+11.8253P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                2592
_reflns_number_total             3373
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0006504_2.cif
_cod_data_source_block           compound_2
_cod_original_sg_symbol_H-M      'C c c a'
_cod_database_code               4321477
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z'
'-x, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z'
'x, -y, z-1/2'
'-x-1/2, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x, y+1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.21099(2) 0.116898(14) 0.33339(3) 0.03509(19) Uani 1 1 d . . .
C1 C 0.0527(2) 0.12707(15) 0.3636(3) 0.0646(13) Uani 1 1 d . . .
H1 H 0.0531 0.1281 0.2986 0.078 Uiso 1 1 calc R . .
C2 C -0.0114(2) 0.12334(16) 0.4081(3) 0.0728(15) Uani 1 1 d . . .
H2 H -0.0526 0.1211 0.3736 0.087 Uiso 1 1 calc R . .
C3 C -0.01308(19) 0.12301(12) 0.5036(3) 0.0522(11) Uani 1 1 d . . .
H3 H -0.0556 0.1206 0.5351 0.063 Uiso 1 1 calc R . .
C4 C 0.04933(17) 0.12636(10) 0.5529(2) 0.0359(8) Uani 1 1 d . . .
C5 C 0.11132(18) 0.12935(10) 0.5026(3) 0.0366(8) Uani 1 1 d . . .
H5 H 0.1533 0.1315 0.5356 0.044 Uiso 1 1 calc R . .
C6 C 0.05093(19) 0.12576(10) 0.6547(2) 0.0386(9) Uani 1 1 d . . .
H6 H 0.0938 0.1266 0.6858 0.046 Uiso 1 1 calc R . .
C7 C 0.2133(2) 0.20684(12) 0.3707(3) 0.0501(10) Uani 1 1 d . . .
H7 H 0.1648 0.2033 0.3713 0.060 Uiso 1 1 calc R . .
C8 C 0.2391(2) 0.24493(12) 0.3785(3) 0.0583(12) Uani 1 1 d . . .
H8 H 0.2085 0.2664 0.3832 0.070 Uiso 1 1 calc R . .
C9 C 0.3101(2) 0.25084(12) 0.3792(3) 0.0538(11) Uani 1 1 d . . .
H9 H 0.3287 0.2763 0.3852 0.065 Uiso 1 1 calc R . .
C10 C 0.35394(19) 0.21803(10) 0.3708(3) 0.0410(9) Uani 1 1 d . . .
C11 C 0.32334(19) 0.18068(10) 0.3623(2) 0.0397(9) Uani 1 1 d . . .
H11 H 0.3527 0.1587 0.3564 0.048 Uiso 1 1 calc R . .
C12 C 0.4306(2) 0.22019(11) 0.3710(3) 0.0519(11) Uani 1 1 d . . .
H12 H 0.4564 0.1968 0.3648 0.062 Uiso 1 1 calc R . .
C13 C 0.1796(2) 0.04325(12) 0.2101(3) 0.0549(11) Uani 1 1 d . . .
H13 H 0.2078 0.0563 0.1667 0.066 Uiso 1 1 calc R . .
C14 C 0.1497(3) 0.00734(13) 0.1853(3) 0.0697(13) Uani 1 1 d . . .
H14 H 0.1585 -0.0038 0.1269 0.084 Uiso 1 1 calc R . .
C15 C 0.1068(2) -0.01165(13) 0.2483(4) 0.0683(13) Uani 1 1 d . . .
H15 H 0.0863 -0.0359 0.2332 0.082 Uiso 1 1 calc R . .
C16 C 0.0943(2) 0.00557(11) 0.3342(3) 0.0518(11) Uani 1 1 d . . .
C17 C 0.1287(2) 0.04093(12) 0.3545(3) 0.0524(11) Uani 1 1 d . . .
H17 H 0.1228 0.0520 0.4136 0.063 Uiso 1 1 calc R . .
C18 C 0.0450(2) -0.01068(13) 0.4032(3) 0.0593(12) Uani 1 1 d . . .
H18 H 0.0287 -0.0366 0.3967 0.071 Uiso 1 1 calc R . .
N1 N 0.11398(14) 0.12928(9) 0.40841(19) 0.0385(7) Uani 1 1 d . . .
N2 N -0.00566(16) 0.12410(9) 0.7013(2) 0.0435(8) Uani 1 1 d . . .
N3 N 0.25391(15) 0.17462(8) 0.3623(2) 0.0362(7) Uani 1 1 d . . .
N4 N 0.46299(17) 0.25263(10) 0.3793(3) 0.0666(11) Uani 1 1 d . . .
N5 N 0.16982(16) 0.05984(9) 0.2934(2) 0.0455(8) Uani 1 1 d . . .
N6 N 0.02415(18) 0.01029(11) 0.4717(3) 0.0657(11) Uani 1 1 d . . .
N7 N 0.30067(19) 0.07785(10) 0.4406(3) 0.0568(9) Uani 1 1 d . . .
N8 N 0.21362(19) 0.14448(10) 0.1577(2) 0.0467(8) Uani 1 1 d . . .
O1 O 0.24073(16) 0.08594(10) 0.4684(2) 0.0712(9) Uani 1 1 d . . .
O2 O 0.34402(18) 0.06047(11) 0.4885(3) 0.0908(12) Uani 1 1 d . . .
O3 O 0.31515(16) 0.08958(9) 0.3590(3) 0.0667(9) Uani 1 1 d . . .
O4 O 0.16109(13) 0.14319(9) 0.21125(18) 0.0528(7) Uani 1 1 d . . .
O5 O 0.26743(16) 0.12737(10) 0.1907(2) 0.0693(9) Uani 1 1 d . . .
O6 O 0.2110(2) 0.15958(9) 0.0819(2) 0.0894(12) Uani 1 1 d . . .
O7A O 0.023(2) 0.2678(6) 0.3562(17) 0.150(10) Uani 0.33 1 d P . .
O7B O 0.0516(9) 0.2768(6) 0.276(2) 0.142(6) Uani 0.33 1 d P . .
O7C O -0.0280(13) 0.2635(14) 0.308(3) 0.21(2) Uani 0.33 1 d P . .
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
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Co N5 175.63(11) . . ?
N3 Co N1 93.15(11) . . ?
N5 Co N1 89.58(12) . . ?
N3 Co O4 87.31(11) . . ?
N5 Co O4 89.44(11) . . ?
N1 Co O4 87.00(10) . . ?
N3 Co O3 90.15(11) . . ?
N5 Co O3 90.00(12) . . ?
N1 Co O3 139.22(12) . . ?
O4 Co O3 133.78(12) . . ?
N3 Co O1 99.02(11) . . ?
N5 Co O1 84.69(12) . . ?
N1 Co O1 83.10(11) . . ?
O4 Co O1 168.51(11) . . ?
O3 Co O1 56.27(11) . . ?
N3 Co O5 81.74(11) . . ?
N5 Co O5 94.02(12) . . ?
N1 Co O5 142.49(12) . . ?
O4 Co O5 55.77(11) . . ?
O3 Co O5 78.18(13) . . ?
O1 Co O5 134.41(12) . . ?
N1 C1 C2 123.8(4) . . ?
C3 C2 C1 118.8(4) . . ?
C2 C3 C4 119.2(4) . . ?
C5 C4 C3 118.1(3) . . ?
C5 C4 C6 120.1(3) . . ?
C3 C4 C6 121.7(3) . . ?
N1 C5 C4 123.4(3) . . ?
N2 C6 C4 120.5(3) . . ?
N3 C7 C8 123.7(4) . . ?
C9 C8 C7 119.3(4) . . ?
C8 C9 C10 118.6(4) . . ?
C9 C10 C11 118.3(3) . . ?
C9 C10 C12 124.1(3) . . ?
C11 C10 C12 117.6(3) . . ?
N3 C11 C10 123.5(3) . . ?
N4 C12 C10 122.1(4) . . ?
N5 C13 C14 122.6(4) . . ?
C15 C14 C13 118.9(4) . . ?
C14 C15 C16 119.4(4) . . ?
C15 C16 C17 117.7(4) . . ?
C15 C16 C18 123.5(4) . . ?
C17 C16 C18 118.7(4) . . ?
N5 C17 C16 123.2(4) . . ?
N6 C18 C16 120.7(4) . . ?
C1 N1 C5 116.6(3) . . ?
C1 N1 Co 119.7(2) . . ?
C5 N1 Co 121.7(2) . . ?
C6 N2 N2 112.9(4) . 3_556 ?
C7 N3 C11 116.6(3) . . ?
C7 N3 Co 122.0(2) . . ?
C11 N3 Co 121.0(2) . . ?
C12 N4 N4 112.2(4) . 6 ?
C13 N5 C17 118.0(3) . . ?
C13 N5 Co 124.2(3) . . ?
C17 N5 Co 117.7(3) . . ?
C18 N6 N6 112.0(5) . 9_556 ?
O2 N7 O1 123.2(4) . . ?
O2 N7 O3 121.4(4) . . ?
O1 N7 O3 115.4(4) . . ?
O6 N8 O4 122.1(4) . . ?
O6 N8 O5 124.3(4) . . ?
O4 N8 O5 113.5(3) . . ?
N7 O1 Co 93.3(3) . . ?
N7 O3 Co 95.0(2) . . ?
N8 O4 Co 99.0(2) . . ?
N8 O5 Co 91.3(2) . . ?
O7C O7A O7C 69(2) . 6_455 ?
O7C O7A O7B 82(3) . . ?
O7C O7A O7B 72(2) 6_455 . ?
O7C O7A O7A 55(2) . 6_455 ?
O7C O7A O7A 50.9(15) 6_455 6_455 ?
O7B O7A O7A 115.7(14) . 6_455 ?
O7A O7B O7C 124(2) . 3 ?
O7A O7B O7C 53.0(19) . 6_455 ?
O7C O7B O7C 83(2) 3 6_455 ?
O7A O7B O7C 46(2) . . ?
O7C O7B O7C 82(2) 3 . ?
O7C O7B O7C 53(2) 6_455 . ?
O7A O7C O7A 74(3) . 6_455 ?
O7A O7C O7B 137(4) . 3 ?
O7A O7C O7B 141(4) 6_455 3 ?
O7A O7C O7C 57.6(16) . 6_455 ?
O7A O7C O7C 53.0(16) 6_455 6_455 ?
O7B O7C O7C 117.6(10) 3 6_455 ?
O7A O7C O7B 122(4) . 6_455 ?
O7A O7C O7B 55(3) 6_455 6_455 ?
O7B O7C O7B 86(2) 3 6_455 ?
O7C O7C O7B 69(4) 6_455 6_455 ?
O7A O7C O7B 51.7(15) . . ?
O7A O7C O7B 108(3) 6_455 . ?
O7B O7C O7B 88(3) 3 . ?
O7C O7C O7B 58(3) 6_455 . ?
O7B O7C O7B 116.0(19) 6_455 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co N3 2.146(3) . ?
Co N5 2.150(3) . ?
Co N1 2.175(3) . ?
Co O4 2.176(3) . ?
Co O3 2.215(3) . ?
Co O1 2.265(3) . ?
Co O5 2.332(3) . ?
C1 N1 1.333(5) . ?
C1 C2 1.380(6) . ?
C2 C3 1.366(6) . ?
C3 C4 1.386(5) . ?
C4 C5 1.385(5) . ?
C4 C6 1.456(5) . ?
C5 N1 1.348(4) . ?
C6 N2 1.268(5) . ?
C7 N3 1.336(5) . ?
C7 C8 1.376(6) . ?
C8 C9 1.365(6) . ?
C9 C10 1.388(5) . ?
C10 C11 1.390(5) . ?
C10 C12 1.461(5) . ?
C11 N3 1.337(4) . ?
C12 N4 1.259(5) . ?
C13 N5 1.329(5) . ?
C13 C14 1.381(6) . ?
C14 C15 1.374(6) . ?
C15 C16 1.378(6) . ?
C16 C17 1.388(5) . ?
C16 C18 1.469(6) . ?
C17 N5 1.334(5) . ?
C18 N6 1.270(6) . ?
N2 N2 1.410(6) 3_556 ?
N4 N4 1.420(7) 6 ?
N6 N6 1.407(6) 9_556 ?
N7 O2 1.222(4) . ?
N7 O1 1.238(4) . ?
N7 O3 1.261(5) . ?
N8 O6 1.198(4) . ?
N8 O4 1.260(4) . ?
N8 O5 1.266(4) . ?
O7A O7C 1.19(3) . ?
O7A O7C 1.26(5) 6_455 ?
O7A O7B 1.30(3) . ?
O7A O7A 1.48(5) 6_455 ?
O7B O7C 1.36(3) 3 ?
O7B O7C 1.50(5) 6_455 ?
O7B O7C 1.64(4) . ?
O7C O7A 1.26(5) 6_455 ?
O7C O7B 1.36(3) 3 ?
O7C O7C 1.40(5) 6_455 ?
O7C O7B 1.50(5) 6_455 ?
