#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/83/2228382.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_2228382
loop_
_publ_author_name
'Zhang, Daopeng'
_publ_section_title
;
 Bis(4-chloropyridine){2,2'-[ethane-1,2-diylbis(nitrilomethylidyne)]diphenolato}cobalt(III)
 perchlorate methanol monosolvate
;
_journal_coeditor_code           HG2742
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1633
_journal_paper_doi               10.1107/S1600536810047793
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Co (C16 H14 N2 O2) (C5 H4 Cl N)2] Cl O4, C H4 O'
_chemical_formula_moiety         'C26 H22 Cl2 Co N4 O2 +, Cl O4 -, C H4 O'
_chemical_formula_sum            'C27 H26 Cl3 Co N4 O7'
_chemical_formula_weight         683.80
_chemical_name_systematic
;
Bis(4-chloropyridine){2,2'-[ethane-1,2-
diylbis(nitrilomethylidyne)]diphenolato}cobalt(III)
perchlorate methanol monosolvate
;
_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                92.757(2)
_cell_angle_beta                 103.843(2)
_cell_angle_gamma                95.396(2)
_cell_formula_units_Z            2
_cell_length_a                   9.0244(12)
_cell_length_b                   11.2625(16)
_cell_length_c                   15.052(2)
_cell_measurement_reflns_used    1564
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.861
_cell_measurement_theta_min      2.678
_cell_volume                     1474.9(3)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008b)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7378
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.8053
_exptl_absorpt_correction_T_min  0.7666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008a)'
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.207
_refine_diff_density_min         -0.494
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         5144
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0523
_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)+(0.0871P)²+1.6441P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1599
_reflns_number_gt                4213
_reflns_number_total             5144
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hg2742.cif
_cod_data_source_block           I
_cod_database_code               2228382
_cod_database_fobs_code          2228382
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 Co1 0.86908(5) 0.11688(4) 0.27546(3) 0.03389(18) Uani d . 1 . .
Cl Cl1 0.7528(2) -0.42638(12) 0.38879(11) 0.0922(5) Uani d . 1 . .
Cl Cl2 1.12614(17) 0.66668(11) 0.25101(11) 0.0786(4) Uani d . 1 . .
Cl Cl3 0.18397(16) 0.27636(12) 0.02468(9) 0.0665(3) Uani d . 1 . .
O O1 1.0710(3) 0.1026(2) 0.34504(16) 0.0395(6) Uani d . 1 . .
O O2 0.8300(3) 0.1686(2) 0.38825(16) 0.0390(6) Uani d . 1 . .
O O3 0.0318(7) 0.2275(8) -0.0063(5) 0.186(3) Uani d . 1 . .
O O4 0.2366(8) 0.3413(8) -0.0360(5) 0.178(3) Uani d . 1 . .
O O5 0.2650(11) 0.1777(7) 0.0309(7) 0.222(4) Uani d . 1 . .
O O6 0.2264(10) 0.3178(9) 0.1133(4) 0.205(4) Uani d . 1 . .
O O7 0.5606(10) 0.2638(9) 0.9505(7) 0.221(5) Uani d . 1 . .
H H7 0.5417 0.2768 1.0005 0.332 Uiso d R 1 . .
N N1 0.9058(4) 0.0653(3) 0.1619(2) 0.0401(7) Uani d . 1 . .
N N2 0.6671(3) 0.1307(3) 0.2060(2) 0.0374(7) Uani d . 1 . .
N N3 0.8215(3) -0.0521(3) 0.3026(2) 0.0384(7) Uani d . 1 . .
N N4 0.9340(3) 0.2864(3) 0.2621(2) 0.0390(7) Uani d . 1 . .
C C1 1.1544(4) -0.0002(3) 0.2244(3) 0.0397(8) Uani d . 1 . .
C C2 1.1695(4) 0.0401(3) 0.3167(2) 0.0357(8) Uani d . 1 . .
C C3 1.2979(4) 0.0125(4) 0.3825(3) 0.0471(9) Uani d . 1 . .
H H3 1.3099 0.0375 0.4438 0.056 Uiso calc R 1 . .
C C4 1.4067(5) -0.0514(4) 0.3574(3) 0.0563(11) Uani d . 1 . .
H H4 1.4909 -0.0687 0.4022 0.068 Uiso calc R 1 . .
C C5 1.3924(5) -0.0902(4) 0.2664(3) 0.0554(11) Uani d . 1 . .
H H5 1.4667 -0.1327 0.2502 0.066 Uiso calc R 1 . .
C C6 1.2690(5) -0.0655(4) 0.2015(3) 0.0511(10) Uani d . 1 . .
H H6 1.2590 -0.0918 0.1407 0.061 Uiso calc R 1 . .
C C7 1.0261(5) 0.0194(4) 0.1520(3) 0.0448(9) Uani d . 1 . .
H H7A 1.0303 -0.0031 0.0924 0.054 Uiso calc R 1 . .
C C8 0.5817(4) 0.2362(3) 0.3251(3) 0.0392(8) Uani d . 1 . .
C C9 0.7113(4) 0.2225(3) 0.3977(2) 0.0358(8) Uani d . 1 . .
C C10 0.7089(5) 0.2673(4) 0.4864(3) 0.0456(9) Uani d . 1 . .
H H10 0.7915 0.2589 0.5354 0.055 Uiso calc R 1 . .
C C11 0.5884(5) 0.3226(4) 0.5022(3) 0.0516(10) Uani d . 1 . .
H H11 0.5900 0.3504 0.5616 0.062 Uiso calc R 1 . .
C C12 0.4637(5) 0.3381(4) 0.4310(3) 0.0577(11) Uani d . 1 . .
H H12 0.3831 0.3773 0.4423 0.069 Uiso calc R 1 . .
C C13 0.4607(5) 0.2947(4) 0.3435(3) 0.0509(10) Uani d . 1 . .
H H13 0.3768 0.3043 0.2957 0.061 Uiso calc R 1 . .
C C14 0.5654(4) 0.1835(3) 0.2337(3) 0.0413(9) Uani d . 1 . .
H H14 0.4729 0.1884 0.1912 0.050 Uiso calc R 1 . .
C C15 0.7786(5) 0.0764(4) 0.0805(3) 0.0520(11) Uani d . 1 . .
H H15A 0.7719 0.0110 0.0348 0.062 Uiso calc R 1 . .
H H15B 0.7967 0.1511 0.0533 0.062 Uiso calc R 1 . .
C C16 0.6310(5) 0.0731(4) 0.1120(3) 0.0495(10) Uani d . 1 . .
H H16A 0.5571 0.1153 0.0711 0.059 Uiso calc R 1 . .
H H16B 0.5870 -0.0090 0.1114 0.059 Uiso calc R 1 . .
C C17 0.7805(5) -0.1467(4) 0.2413(3) 0.0454(9) Uani d . 1 . .
H H17 0.7667 -0.1333 0.1795 0.055 Uiso calc R 1 . .
C C18 0.7576(5) -0.2624(4) 0.2642(3) 0.0541(11) Uani d . 1 . .
H H18 0.7278 -0.3253 0.2192 0.065 Uiso calc R 1 . .
C C19 0.7798(5) -0.2828(4) 0.3555(3) 0.0534(11) Uani d . 1 . .
C C20 0.8241(6) -0.1875(4) 0.4200(3) 0.0570(11) Uani d . 1 . .
H H20 0.8399 -0.1992 0.4822 0.068 Uiso calc R 1 . .
C C21 0.8445(5) -0.0751(4) 0.3914(3) 0.0470(9) Uani d . 1 . .
H H21 0.8760 -0.0113 0.4356 0.056 Uiso calc R 1 . .
C C22 0.8877(5) 0.3475(4) 0.1886(3) 0.0533(11) Uani d . 1 . .
H H22 0.8144 0.3090 0.1388 0.064 Uiso calc R 1 . .
C C23 0.9419(6) 0.4633(4) 0.1823(3) 0.0620(12) Uani d . 1 . .
H H23 0.9067 0.5022 0.1294 0.074 Uiso calc R 1 . .
C C24 1.0492(5) 0.5210(4) 0.2553(3) 0.0522(10) Uani d . 1 . .
C C25 1.0946(5) 0.4621(4) 0.3331(3) 0.0609(12) Uani d . 1 . .
H H25 1.1642 0.5003 0.3846 0.073 Uiso calc R 1 . .
C C26 1.0355(5) 0.3463(4) 0.3333(3) 0.0548(11) Uani d . 1 . .
H H26 1.0676 0.3066 0.3862 0.066 Uiso calc R 1 . .
C C27 0.6289(12) 0.3621(9) 0.9273(7) 0.150(4) Uani d . 1 . .
H H27A 0.6190 0.4289 0.9666 0.225 Uiso calc R 1 . .
H H27B 0.5819 0.3752 0.8647 0.225 Uiso calc R 1 . .
H H27C 0.7357 0.3537 0.9335 0.225 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'
Cl Cl 0.1484 0.1585 '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
O2 Co1 N1 . . 179.33(12) ?
O2 Co1 N2 . . 94.28(12) ?
N1 Co1 N2 . . 85.06(13) ?
O2 Co1 O1 . . 85.71(10) ?
N1 Co1 O1 . . 94.95(12) ?
N2 Co1 O1 . . 179.83(13) ?
O2 Co1 N4 . . 87.07(12) ?
N1 Co1 N4 . . 92.94(13) ?
N2 Co1 N4 . . 91.30(13) ?
O1 Co1 N4 . . 88.86(12) ?
O2 Co1 N3 . . 89.24(12) ?
N1 Co1 N3 . . 90.81(13) ?
N2 Co1 N3 . . 94.37(13) ?
O1 Co1 N3 . . 85.46(12) ?
N4 Co1 N3 . . 173.45(12) ?
O4 Cl3 O6 . . 117.6(6) ?
O4 Cl3 O5 . . 104.2(7) ?
O6 Cl3 O5 . . 98.6(6) ?
O4 Cl3 O3 . . 114.2(5) ?
O6 Cl3 O3 . . 115.2(5) ?
O5 Cl3 O3 . . 103.6(6) ?
C2 O1 Co1 . . 124.5(2) ?
C9 O2 Co1 . . 125.6(2) ?
C27 O7 H7 . . 109.5 ?
C7 N1 C15 . . 119.9(3) ?
C7 N1 Co1 . . 125.3(3) ?
C15 N1 Co1 . . 114.8(2) ?
C14 N2 C16 . . 119.9(3) ?
C14 N2 Co1 . . 126.0(3) ?
C16 N2 Co1 . . 114.1(2) ?
C17 N3 C21 . . 116.5(3) ?
C17 N3 Co1 . . 126.2(3) ?
C21 N3 Co1 . . 117.1(3) ?
C22 N4 C26 . . 116.2(4) ?
C22 N4 Co1 . . 126.6(3) ?
C26 N4 Co1 . . 117.2(3) ?
C2 C1 C6 . . 119.3(4) ?
C2 C1 C7 . . 122.9(3) ?
C6 C1 C7 . . 117.8(4) ?
O1 C2 C3 . . 117.9(3) ?
O1 C2 C1 . . 124.1(3) ?
C3 C2 C1 . . 118.0(3) ?
C4 C3 C2 . . 120.9(4) ?
C4 C3 H3 . . 119.5 ?
C2 C3 H3 . . 119.5 ?
C3 C4 C5 . . 121.1(4) ?
C3 C4 H4 . . 119.5 ?
C5 C4 H4 . . 119.5 ?
C6 C5 C4 . . 119.2(4) ?
C6 C5 H5 . . 120.4 ?
C4 C5 H5 . . 120.4 ?
C5 C6 C1 . . 121.5(4) ?
C5 C6 H6 . . 119.3 ?
C1 C6 H6 . . 119.3 ?
N1 C7 C1 . . 125.7(3) ?
N1 C7 H7A . . 117.2 ?
C1 C7 H7A . . 117.2 ?
C13 C8 C9 . . 119.7(4) ?
C13 C8 C14 . . 118.4(3) ?
C9 C8 C14 . . 121.7(3) ?
O2 C9 C10 . . 118.1(3) ?
O2 C9 C8 . . 124.7(3) ?
C10 C9 C8 . . 117.2(3) ?
C11 C10 C9 . . 121.7(4) ?
C11 C10 H10 . . 119.2 ?
C9 C10 H10 . . 119.2 ?
C10 C11 C12 . . 121.1(4) ?
C10 C11 H11 . . 119.5 ?
C12 C11 H11 . . 119.5 ?
C13 C12 C11 . . 119.2(4) ?
C13 C12 H12 . . 120.4 ?
C11 C12 H12 . . 120.4 ?
C12 C13 C8 . . 121.3(4) ?
C12 C13 H13 . . 119.4 ?
C8 C13 H13 . . 119.4 ?
N2 C14 C8 . . 125.6(3) ?
N2 C14 H14 . . 117.2 ?
C8 C14 H14 . . 117.2 ?
N1 C15 C16 . . 107.9(3) ?
N1 C15 H15A . . 110.1 ?
C16 C15 H15A . . 110.1 ?
N1 C15 H15B . . 110.1 ?
C16 C15 H15B . . 110.1 ?
H15A C15 H15B . . 108.4 ?
N2 C16 C15 . . 108.2(3) ?
N2 C16 H16A . . 110.1 ?
C15 C16 H16A . . 110.1 ?
N2 C16 H16B . . 110.1 ?
C15 C16 H16B . . 110.1 ?
H16A C16 H16B . . 108.4 ?
N3 C17 C18 . . 123.9(4) ?
N3 C17 H17 . . 118.1 ?
C18 C17 H17 . . 118.1 ?
C17 C18 C19 . . 118.3(4) ?
C17 C18 H18 . . 120.8 ?
C19 C18 H18 . . 120.8 ?
C18 C19 C20 . . 119.0(4) ?
C18 C19 Cl1 . . 120.5(4) ?
C20 C19 Cl1 . . 120.4(4) ?
C21 C20 C19 . . 119.0(4) ?
C21 C20 H20 . . 120.5 ?
C19 C20 H20 . . 120.5 ?
N3 C21 C20 . . 123.3(4) ?
N3 C21 H21 . . 118.3 ?
C20 C21 H21 . . 118.3 ?
N4 C22 C23 . . 123.7(4) ?
N4 C22 H22 . . 118.1 ?
C23 C22 H22 . . 118.1 ?
C22 C23 C24 . . 118.7(4) ?
C22 C23 H23 . . 120.7 ?
C24 C23 H23 . . 120.7 ?
C23 C24 C25 . . 119.0(4) ?
C23 C24 Cl2 . . 121.1(3) ?
C25 C24 Cl2 . . 119.9(4) ?
C26 C25 C24 . . 118.5(4) ?
C26 C25 H25 . . 120.7 ?
C24 C25 H25 . . 120.7 ?
N4 C26 C25 . . 123.9(4) ?
N4 C26 H26 . . 118.1 ?
C25 C26 H26 . . 118.1 ?
O7 C27 H27A . . 109.5 ?
O7 C27 H27B . . 109.5 ?
H27A C27 H27B . . 109.5 ?
O7 C27 H27C . . 109.5 ?
H27A C27 H27C . . 109.5 ?
H27B C27 H27C . . 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 O2 . 1.891(2) ?
Co1 N1 . 1.892(3) ?
Co1 N2 . 1.897(3) ?
Co1 O1 . 1.898(2) ?
Co1 N4 . 1.977(3) ?
Co1 N3 . 1.995(3) ?
Cl1 C19 . 1.728(4) ?
Cl2 C24 . 1.730(4) ?
Cl3 O4 . 1.342(6) ?
Cl3 O6 . 1.344(6) ?
Cl3 O5 . 1.382(7) ?
Cl3 O3 . 1.391(6) ?
O1 C2 . 1.318(4) ?
O2 C9 . 1.312(4) ?
O7 C27 . 1.319(10) ?
O7 H7 . 0.8200 ?
N1 C7 . 1.282(5) ?
N1 C15 . 1.485(5) ?
N2 C14 . 1.278(5) ?
N2 C16 . 1.477(5) ?
N3 C17 . 1.339(5) ?
N3 C21 . 1.344(5) ?
N4 C22 . 1.334(5) ?
N4 C26 . 1.337(5) ?
C1 C2 . 1.412(5) ?
C1 C6 . 1.420(5) ?
C1 C7 . 1.430(5) ?
C2 C3 . 1.403(5) ?
C3 C4 . 1.381(6) ?
C3 H3 . 0.9300 ?
C4 C5 . 1.390(7) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.355(6) ?
C5 H5 . 0.9300 ?
C6 H6 . 0.9300 ?
C7 H7A . 0.9300 ?
C8 C13 . 1.402(5) ?
C8 C9 . 1.423(5) ?
C8 C14 . 1.440(5) ?
C9 C10 . 1.410(5) ?
C10 C11 . 1.365(6) ?
C10 H10 . 0.9300 ?
C11 C12 . 1.387(6) ?
C11 H11 . 0.9300 ?
C12 C13 . 1.376(6) ?
C12 H12 . 0.9300 ?
C13 H13 . 0.9300 ?
C14 H14 . 0.9300 ?
C15 C16 . 1.515(6) ?
C15 H15A . 0.9700 ?
C15 H15B . 0.9700 ?
C16 H16A . 0.9700 ?
C16 H16B . 0.9700 ?
C17 C18 . 1.373(6) ?
C17 H17 . 0.9300 ?
C18 C19 . 1.374(6) ?
C18 H18 . 0.9300 ?
C19 C20 . 1.375(6) ?
C20 C21 . 1.366(6) ?
C20 H20 . 0.9300 ?
C21 H21 . 0.9300 ?
C22 C23 . 1.365(6) ?
C22 H22 . 0.9300 ?
C23 C24 . 1.369(6) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.369(6) ?
C25 C26 . 1.363(6) ?
C25 H25 . 0.9300 ?
C26 H26 . 0.9300 ?
C27 H27A . 0.9600 ?
C27 H27B . 0.9600 ?
C27 H27C . 0.9600 ?
