#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:24:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179448 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/45/4334568.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_4334568
loop_
_publ_author_name
'Anuj Kumar Sharma'
'Francesc Lloret'
'Rabindranath Mukherjee'
_publ_contact_author
; Rabindranath Mukherjee
  Department of Chemistry
  Indian Institute of Technology
  Kanpur 208016
  INDIA
;
_publ_contact_author_email       rnm@iitk.ac.in
_publ_contact_author_fax         '+91 (512) 2597437'
_publ_contact_author_phone       '+91 (512) 2597437'
_publ_section_title
;
 Phenolate- and Acetate (Both μ2-1,1 and μ2-1,3 Modes)-Bridged Linear
 CoII3 and CoII2MnII Trimers: Magnetostructural Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4825
_journal_page_last               4833
_journal_paper_doi               10.1021/ic302259t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C46 H60 Co2 Mn N4 O18'
_chemical_formula_sum            'C46 H60 Co2 Mn N4 O18'
_chemical_formula_weight         1129.78
_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                79.839(5)
_cell_angle_beta                 82.283(5)
_cell_angle_gamma                85.919(5)
_cell_formula_units_Z            1
_cell_length_a                   9.454(5)
_cell_length_b                   11.068(5)
_cell_length_c                   13.418(5)
_cell_measurement_temperature    100(2)
_cell_volume                     1367.9(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, et. al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9054
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.8410
_exptl_absorpt_correction_T_min  0.7746
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Pink
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       Block
_exptl_crystal_F_000             587
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         6428
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0537
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0382P)²+6.1671P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1627
_reflns_number_gt                5315
_reflns_number_total             6428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302259t_si_002_3.cif
_cod_data_source_block           Co2Mn
_cod_database_code               4334568
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.60154(5) 0.62177(5) 0.67502(4) 0.01596(14) Uani 1 1 d . . .
Mn Mn 0.5000 0.5000 0.5000 0.01234(17) Uani 1 2 d S . .
O1 O 0.4549(3) 0.6508(2) 0.57720(19) 0.0163(5) Uani 1 1 d . . .
O2 O 0.7646(3) 0.6649(3) 0.5552(2) 0.0197(6) Uani 1 1 d . . .
O3 O 0.6881(3) 0.5846(3) 0.4307(2) 0.0206(6) Uani 1 1 d . . .
O4 O 0.6038(3) 0.4367(2) 0.63795(19) 0.0177(5) Uani 1 1 d . . .
O5 O 0.6772(4) 0.3290(3) 0.7786(2) 0.0313(7) Uani 1 1 d . . .
O6 O 0.7566(3) 0.5509(3) 0.7756(2) 0.0224(6) Uani 1 1 d . . .
N1 N 0.4383(4) 0.5740(3) 0.8031(2) 0.0198(7) Uani 1 1 d . . .
N2 N 0.5871(3) 0.8096(3) 0.7035(2) 0.0174(6) Uani 1 1 d . . .
C1 C 0.3451(4) 0.4902(4) 0.7977(3) 0.0199(8) Uani 1 1 d . . .
H1 H 0.3489 0.4586 0.7359 0.024 Uiso 1 1 calc R . .
C2 C 0.2441(4) 0.4478(4) 0.8778(3) 0.0244(8) Uani 1 1 d . . .
H2 H 0.1803 0.3879 0.8712 0.029 Uiso 1 1 calc R . .
C3 C 0.2367(5) 0.4937(4) 0.9678(3) 0.0256(9) Uani 1 1 d . . .
H3 H 0.1697 0.4646 1.0249 0.031 Uiso 1 1 calc R . .
C4 C 0.3297(5) 0.5833(4) 0.9725(3) 0.0255(9) Uani 1 1 d . . .
H4 H 0.3249 0.6183 1.0328 0.031 Uiso 1 1 calc R . .
C5 C 0.4292(4) 0.6220(4) 0.8900(3) 0.0206(8) Uani 1 1 d . . .
C6 C 0.5226(5) 0.7265(4) 0.8895(3) 0.0225(8) Uani 1 1 d . . .
H6A H 0.6241 0.6964 0.8835 0.027 Uiso 1 1 calc R . .
H6B H 0.5001 0.7578 0.9549 0.027 Uiso 1 1 calc R . .
C7 C 0.5004(4) 0.8308(4) 0.8011(3) 0.0234(8) Uani 1 1 d . . .
H7A H 0.3979 0.8392 0.7914 0.028 Uiso 1 1 calc R . .
H7B H 0.5268 0.9088 0.8185 0.028 Uiso 1 1 calc R . .
C8 C 0.7335(4) 0.8515(4) 0.7020(3) 0.0237(8) Uani 1 1 d . . .
H8A H 0.7919 0.8380 0.6385 0.035 Uiso 1 1 calc R . .
H8B H 0.7769 0.8050 0.7603 0.035 Uiso 1 1 calc R . .
H8C H 0.7283 0.9393 0.7061 0.035 Uiso 1 1 calc R . .
C9 C 0.5250(4) 0.8846(3) 0.6150(3) 0.0198(8) Uani 1 1 d . . .
H9A H 0.5878 0.8733 0.5517 0.024 Uiso 1 1 calc R . .
H9B H 0.5245 0.9724 0.6213 0.024 Uiso 1 1 calc R . .
C10 C 0.3755(4) 0.8542(4) 0.6045(3) 0.0193(7) Uani 1 1 d . . .
C11 C 0.2642(4) 0.9426(4) 0.6080(3) 0.0246(8) Uani 1 1 d . . .
H11 H 0.2824 1.0207 0.6225 0.030 Uiso 1 1 calc R . .
C12 C 0.1280(4) 0.9212(4) 0.5911(3) 0.0253(9) Uani 1 1 d . . .
H12 H 0.0541 0.9839 0.5925 0.030 Uiso 1 1 calc R . .
C13 C 0.1009(4) 0.8054(4) 0.5718(3) 0.0258(9) Uani 1 1 d . . .
H13 H 0.0075 0.7886 0.5612 0.031 Uiso 1 1 calc R . .
C14 C 0.2097(4) 0.7152(4) 0.5683(3) 0.0202(8) Uani 1 1 d . . .
H14 H 0.1901 0.6370 0.5549 0.024 Uiso 1 1 calc R . .
C15 C 0.3488(4) 0.7377(3) 0.5842(3) 0.0169(7) Uani 1 1 d . . .
C16 C 0.7712(4) 0.6448(4) 0.4651(3) 0.0210(8) Uani 1 1 d . . .
C17 C 0.8953(5) 0.6998(5) 0.3906(4) 0.0337(10) Uani 1 1 d . . .
H17A H 0.8908 0.6785 0.3233 0.051 Uiso 1 1 calc R . .
H17B H 0.9857 0.6668 0.4150 0.051 Uiso 1 1 calc R . .
H17C H 0.8891 0.7894 0.3856 0.051 Uiso 1 1 calc R . .
C18 C 0.6214(4) 0.3350(4) 0.6981(3) 0.0228(8) Uani 1 1 d . . .
C19 C 0.5728(5) 0.2197(4) 0.6727(3) 0.0300(10) Uani 1 1 d . . .
H19A H 0.5313 0.2387 0.6083 0.045 Uiso 1 1 calc R . .
H19B H 0.5007 0.1839 0.7273 0.045 Uiso 1 1 calc R . .
H19C H 0.6546 0.1609 0.6658 0.045 Uiso 1 1 calc R . .
C20 C 0.9088(4) 0.5517(4) 0.7457(4) 0.0291(9) Uani 1 1 d . . .
H20A H 0.9583 0.5147 0.8042 0.044 Uiso 1 1 calc R . .
H20B H 0.9369 0.6366 0.7225 0.044 Uiso 1 1 calc R . .
H20C H 0.9346 0.5044 0.6902 0.044 Uiso 1 1 calc R . .
O1S O 0.7346(4) 0.8997(3) 0.9760(3) 0.0437(9) Uani 1 1 d . . .
O2SA O 0.0472(5) 0.2663(4) 1.0768(3) 0.0396(10) Uiso 0.85 1 d P A 1
O2SB O 0.002(3) 0.227(3) 1.025(2) 0.053(7) Uiso 0.15 1 d P A 2
O3S O 0.7850(5) 0.1318(4) 0.8965(3) 0.0579(12) Uani 1 1 d . . .
C1S C 0.6581(6) 0.8959(5) 1.0749(4) 0.0432(12) Uani 1 1 d . . .
H1S1 H 0.7129 0.9346 1.1168 0.065 Uiso 1 1 calc R . .
H1S2 H 0.6434 0.8103 1.1067 0.065 Uiso 1 1 calc R . .
H1S3 H 0.5652 0.9404 1.0697 0.065 Uiso 1 1 calc R . .
C2S C -0.0653(5) 0.1991(5) 1.1366(4) 0.0411(12) Uani 1 1 d . . .
C3S C 0.9297(8) 0.1499(7) 0.8752(6) 0.0645(18) Uani 1 1 d . . .
H3S1 H 0.9489 0.2305 0.8896 0.097 Uiso 1 1 calc R . .
H3S2 H 0.9610 0.1463 0.8031 0.097 Uiso 1 1 calc R . .
H3S3 H 0.9820 0.0856 0.9179 0.097 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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 '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
O1 Co1 O2 90.79(11) . .
O1 Co1 O6 167.83(11) . .
O2 Co1 O6 90.28(11) . .
O1 Co1 N1 91.29(12) . .
O2 Co1 N1 177.85(12) . .
O6 Co1 N1 87.57(12) . .
O1 Co1 N2 94.72(11) . .
O2 Co1 N2 90.72(12) . .
O6 Co1 N2 97.38(12) . .
N1 Co1 N2 89.65(12) . .
O1 Co1 O4 80.81(10) . .
O2 Co1 O4 89.22(11) . .
O6 Co1 O4 87.09(10) . .
N1 Co1 O4 90.57(11) . .
N2 Co1 O4 175.53(11) . .
O3 Mn O3 180.00(14) . 2_666
O3 Mn O1 87.10(11) . .
O3 Mn O1 92.90(11) 2_666 .
O3 Mn O1 92.90(10) . 2_666
O3 Mn O1 87.10(11) 2_666 2_666
O1 Mn O1 180.00(11) . 2_666
O3 Mn O4 91.07(11) . 2_666
O3 Mn O4 88.93(11) 2_666 2_666
O1 Mn O4 101.44(10) . 2_666
O1 Mn O4 78.56(10) 2_666 2_666
O3 Mn O4 88.93(11) . .
O3 Mn O4 91.07(11) 2_666 .
O1 Mn O4 78.56(10) . .
O1 Mn O4 101.44(10) 2_666 .
O4 Mn O4 180.000(1) 2_666 .
C15 O1 Co1 121.3(2) . .
C15 O1 Mn 136.1(2) . .
Co1 O1 Mn 101.64(11) . .
C16 O2 Co1 127.7(3) . .
C16 O3 Mn 130.9(3) . .
C18 O4 Co1 126.9(2) . .
C18 O4 Mn 136.6(3) . .
Co1 O4 Mn 93.30(10) . .
C20 O6 Co1 123.9(3) . .
C1 N1 C5 118.3(4) . .
C1 N1 Co1 118.8(3) . .
C5 N1 Co1 122.9(3) . .
C8 N2 C9 107.4(3) . .
C8 N2 C7 108.5(3) . .
C9 N2 C7 110.2(3) . .
C8 N2 Co1 109.2(2) . .
C9 N2 Co1 105.6(2) . .
C7 N2 Co1 115.7(2) . .
N1 C1 C2 122.9(4) . .
C1 C2 C3 119.1(4) . .
C2 C3 C4 118.1(4) . .
C5 C4 C3 120.2(4) . .
N1 C5 C4 121.2(4) . .
N1 C5 C6 117.2(3) . .
C4 C5 C6 121.3(4) . .
C5 C6 C7 111.2(3) . .
N2 C7 C6 112.4(3) . .
N2 C9 C10 114.6(3) . .
C11 C10 C15 119.1(4) . .
C11 C10 C9 120.5(4) . .
C15 C10 C9 120.3(3) . .
C12 C11 C10 122.3(4) . .
C11 C12 C13 118.7(4) . .
C14 C13 C12 120.3(4) . .
C13 C14 C15 120.9(4) . .
O1 C15 C14 120.5(3) . .
O1 C15 C10 120.8(3) . .
C14 C15 C10 118.7(3) . .
O3 C16 O2 127.2(4) . .
O3 C16 C17 116.8(4) . .
O2 C16 C17 116.0(4) . .
O5 C18 O4 122.0(4) . .
O5 C18 C19 118.7(4) . .
O4 C18 C19 119.3(4) . .
O2SA C2S O2SB 40.9(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O1 2.006(3) .
Co1 O2 2.088(3) .
Co1 O6 2.140(3) .
Co1 N1 2.167(3) .
Co1 N2 2.171(3) .
Co1 O4 2.189(3) .
Mn O3 2.094(3) .
Mn O3 2.094(3) 2_666
Mn O1 2.105(3) .
Mn O1 2.105(3) 2_666
Mn O4 2.194(3) 2_666
Mn O4 2.194(3) .
O1 C15 1.345(4) .
O2 C16 1.260(5) .
O3 C16 1.247(5) .
O4 C18 1.278(5) .
O5 C18 1.254(5) .
O6 C20 1.440(5) .
N1 C1 1.342(5) .
N1 C5 1.355(5) .
N2 C8 1.487(5) .
N2 C9 1.488(5) .
N2 C7 1.495(5) .
C1 C2 1.377(6) .
C2 C3 1.383(6) .
C3 C4 1.387(6) .
C4 C5 1.380(6) .
C5 C6 1.503(6) .
C6 C7 1.528(6) .
C9 C10 1.506(5) .
C10 C11 1.387(5) .
C10 C15 1.411(5) .
C11 C12 1.382(6) .
C12 C13 1.398(6) .
C13 C14 1.383(6) .
C14 C15 1.406(5) .
C16 C17 1.522(6) .
C18 C19 1.496(6) .
O1S C1S 1.420(6) .
O2SA C2S 1.415(6) .
O2SB C2S 1.54(3) .
O3S C3S 1.381(8) .
