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#$Date: 2016-03-26 21:37:51 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180479 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/48/7214827.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_7214827
loop_
_publ_author_name
'Ding, Cai-Xia'
'Ni, Jia'
'Yang, Yu-Hua'
'Ng, Seik-Weng'
'Wang, Bing-Wu'
'Xie, Yong-Shu'
_publ_section_title
;
 Mono-, Tetra- and octanuclear transition metal complexes of in situ
 generated schiff base ligands containing up to 12 coordinating atoms:
 syntheses, structures and magnetism
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              7312
_journal_paper_doi               10.1039/c2ce25966d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C25 H38 Cl Co N4 O11'
_chemical_formula_weight         664.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 106.2220(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.9687(12)
_cell_length_b                   7.9248(7)
_cell_length_c                   14.4847(14)
_cell_measurement_temperature    293(2)
_cell_volume                     1429.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13170
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_correction_T_min  0.8040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3291
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0607
_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)+(0.0774P)²+2.0095P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1545
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                2574
_reflns_number_total             3291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25966d.txt
_cod_data_source_block           co
_cod_original_sg_symbol_H-M      p2/c
_cod_database_code               7214827
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'-x, -y, -z'
'-x, y, -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
Co1 Co 0.5000 0.72986(8) 0.2500 0.0302(2) Uani 1 2 d S . .
Cl1 Cl 1.0000 0.6545(2) 0.2500 0.0784(6) Uani 1 2 d SD . .
O1 O 0.2180(2) 1.0685(4) 0.1996(2) 0.0557(8) Uani 1 1 d . . .
O2 O 0.3929(2) 0.8989(3) 0.21654(17) 0.0383(6) Uani 1 1 d . . .
O3 O 0.4570(5) 0.1992(7) 0.3200(4) 0.0505(14) Uani 0.50 1 d P A -1
H3A H 0.4390 0.1043 0.2992 0.061 Uiso 0.50 1 calc PR A -1
O4 O 0.9939(10) 0.7288(15) 0.3364(7) 0.117(4) Uani 0.50 1 d PDU B -2
O5 O 0.8949(6) 0.6175(13) 0.1963(7) 0.136(4) Uani 0.50 1 d PDU B -2
O6 O 1.0565(7) 0.5058(10) 0.2706(7) 0.124(4) Uani 0.50 1 d PDU B -2
O7 O 1.0473(9) 0.7640(16) 0.2013(10) 0.182(10) Uani 0.50 1 d PD B -2
O8 O 0.8194(4) 0.5874(8) 0.4078(4) 0.1121(17) Uani 1 1 d . . .
H8 H 0.8709 0.5761 0.3860 0.168 Uiso 1 1 calc R . .
N1 N 0.5237(3) 0.7328(4) 0.1264(2) 0.0402(7) Uani 1 1 d . . .
N2 N 0.6138(2) 0.5591(4) 0.2806(2) 0.0419(7) Uani 1 1 d . . .
H2 H 0.6681 0.6044 0.3282 0.050 Uiso 1 1 calc R . .
C1 C 0.1216(4) 1.1595(7) 0.1930(5) 0.0735(15) Uani 1 1 d . . .
H1A H 0.1138 1.1771 0.2563 0.110 Uiso 1 1 calc R . .
H1B H 0.0614 1.0961 0.1553 0.110 Uiso 1 1 calc R . .
H1C H 0.1245 1.2666 0.1629 0.110 Uiso 1 1 calc R . .
C2 C 0.2400(3) 1.0282(5) 0.1166(3) 0.0447(9) Uani 1 1 d . . .
C3 C 0.1785(4) 1.0721(6) 0.0261(4) 0.0602(12) Uani 1 1 d . . .
H3 H 0.1154 1.1327 0.0191 0.072 Uiso 1 1 calc R . .
C4 C 0.2093(4) 1.0271(7) -0.0548(4) 0.0702(14) Uani 1 1 d . . .
H4 H 0.1664 1.0570 -0.1155 0.084 Uiso 1 1 calc R . .
C5 C 0.3014(4) 0.9402(6) -0.0461(3) 0.0609(12) Uani 1 1 d . . .
H5A H 0.3218 0.9118 -0.1007 0.073 Uiso 1 1 calc R . .
C6 C 0.3664(3) 0.8924(5) 0.0454(3) 0.0414(8) Uani 1 1 d . . .
C7 C 0.3366(3) 0.9352(4) 0.1288(3) 0.0353(7) Uani 1 1 d . . .
C8 C 0.4642(3) 0.8041(5) 0.0509(3) 0.0452(9) Uani 1 1 d . . .
H8A H 0.4862 0.7980 -0.0048 0.054 Uiso 1 1 calc R . .
C9 C 0.6302(4) 0.6667(8) 0.1278(4) 0.0766(17) Uani 1 1 d . . .
H9A H 0.6287 0.6246 0.0646 0.092 Uiso 1 1 calc R . .
H9B H 0.6831 0.7563 0.1446 0.092 Uiso 1 1 calc R . .
C10 C 0.6583(5) 0.5350(7) 0.1960(4) 0.0792(18) Uani 1 1 d . . .
H10A H 0.7360 0.5278 0.2190 0.095 Uiso 1 1 calc R . .
H10B H 0.6320 0.4290 0.1647 0.095 Uiso 1 1 calc R . .
C11 C 0.5888(3) 0.3950(4) 0.3178(3) 0.0415(8) Uani 1 1 d . A .
H11A H 0.5688 0.4151 0.3766 0.050 Uiso 1 1 calc R . .
H11B H 0.6535 0.3271 0.3344 0.050 Uiso 1 1 calc R . .
C12 C 0.5000 0.2939(6) 0.2500 0.0425(12) Uani 1 2 d S . .
H12 H 0.5310 0.2148 0.2131 0.051 Uiso 0.50 1 calc PR A .
C13 C 0.8522(8) 0.5778(12) 0.5027(5) 0.136(4) Uani 1 1 d . . .
H13A H 0.8901 0.6792 0.5282 0.204 Uiso 1 1 calc R . .
H13B H 0.8992 0.4826 0.5214 0.204 Uiso 1 1 calc R . .
H13C H 0.7913 0.5646 0.5274 0.204 Uiso 1 1 calc R . .
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O2 Co1 O2 89.87(16) 4_656 .
O2 Co1 N1 86.11(12) 4_656 .
O2 Co1 N1 92.89(12) . .
O2 Co1 N1 92.89(12) 4_656 4_656
O2 Co1 N1 86.11(12) . 4_656
N1 Co1 N1 178.60(19) . 4_656
O2 Co1 N2 177.50(12) 4_656 4_656
O2 Co1 N2 88.76(12) . 4_656
N1 Co1 N2 96.04(14) . 4_656
N1 Co1 N2 84.94(14) 4_656 4_656
O2 Co1 N2 88.76(12) 4_656 .
O2 Co1 N2 177.50(12) . .
N1 Co1 N2 84.94(14) . .
N1 Co1 N2 96.04(14) 4_656 .
N2 Co1 N2 92.68(18) 4_656 .
O7 Cl1 O7 101.2(13) . 4_756
O7 Cl1 O6 111.6(5) . .
O7 Cl1 O6 136.1(8) 4_756 .
O7 Cl1 O6 136.1(8) . 4_756
O7 Cl1 O6 111.6(5) 4_756 4_756
O6 Cl1 O6 62.1(8) . 4_756
O7 Cl1 O5 110.7(5) . .
O7 Cl1 O5 85.0(7) 4_756 .
O6 Cl1 O5 108.5(5) . .
O6 Cl1 O5 47.4(6) 4_756 .
O7 Cl1 O5 85.0(7) . 4_756
O7 Cl1 O5 110.7(5) 4_756 4_756
O6 Cl1 O5 47.4(6) . 4_756
O6 Cl1 O5 108.5(5) 4_756 4_756
O5 Cl1 O5 155.8(8) . 4_756
O7 Cl1 O4 29.5(8) . 4_756
O7 Cl1 O4 109.8(5) 4_756 4_756
O6 Cl1 O4 113.1(8) . 4_756
O6 Cl1 O4 108.9(5) 4_756 4_756
O5 Cl1 O4 83.2(5) . 4_756
O5 Cl1 O4 107.1(5) 4_756 4_756
O7 Cl1 O4 109.8(5) . .
O7 Cl1 O4 29.5(8) 4_756 .
O6 Cl1 O4 108.9(5) . .
O6 Cl1 O4 113.1(8) 4_756 .
O5 Cl1 O4 107.1(5) . .
O5 Cl1 O4 83.2(5) 4_756 .
O4 Cl1 O4 130.5(11) 4_756 .
C2 O1 C1 117.4(4) . .
C7 O2 Co1 125.1(2) . .
C8 N1 C9 120.6(4) . .
C8 N1 Co1 126.3(3) . .
C9 N1 Co1 112.4(3) . .
C11 N2 C10 111.0(3) . .
C11 N2 Co1 117.5(2) . .
C10 N2 Co1 109.8(3) . .
O1 C2 C3 125.4(4) . .
O1 C2 C7 114.3(3) . .
C3 C2 C7 120.4(4) . .
C2 C3 C4 120.9(4) . .
C5 C4 C3 120.4(4) . .
C4 C5 C6 120.4(5) . .
C7 C6 C5 120.4(4) . .
C7 C6 C8 121.4(3) . .
C5 C6 C8 118.2(4) . .
O2 C7 C6 124.5(3) . .
O2 C7 C2 117.9(3) . .
C6 C7 C2 117.5(3) . .
N1 C8 C6 125.3(4) . .
C10 C9 N1 109.4(4) . .
C9 C10 N2 113.1(4) . .
N2 C11 C12 115.7(3) . .
O3 C12 O3 119.5(6) 4_656 .
O3 C12 C11 110.3(3) 4_656 .
O3 C12 C11 100.7(3) . .
O3 C12 C11 100.7(3) 4_656 4_656
O3 C12 C11 110.3(3) . 4_656
C11 C12 C11 116.2(4) . 4_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O2 1.892(2) 4_656
Co1 O2 1.892(2) .
Co1 N1 1.900(3) .
Co1 N1 1.900(3) 4_656
Co1 N2 1.960(3) 4_656
Co1 N2 1.960(3) .
Cl1 O7 1.367(7) .
Cl1 O7 1.367(7) 4_756
Cl1 O6 1.376(7) .
Cl1 O6 1.376(7) 4_756
Cl1 O5 1.399(7) .
Cl1 O5 1.399(7) 4_756
Cl1 O4 1.405(7) 4_756
Cl1 O4 1.405(7) .
O1 C2 1.349(5) .
O1 C1 1.424(5) .
O2 C7 1.309(4) .
O3 C12 1.490(6) .
O8 C13 1.323(8) .
N1 C8 1.280(5) .
N1 C9 1.471(6) .
N2 C11 1.478(5) .
N2 C10 1.506(6) .
C2 C3 1.375(6) .
C2 C7 1.421(5) .
C3 C4 1.386(7) .
C4 C5 1.353(7) .
C5 C6 1.409(6) .
C6 C7 1.408(5) .
C6 C8 1.431(6) .
C9 C10 1.413(7) .
C11 C12 1.517(5) .
C12 O3 1.490(6) 4_656
C12 C11 1.517(5) 4_656
