#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:24:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179448 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/45/4334570.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_4334570
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         'C38 H46 Mn N4 Ni2 O12'
_chemical_formula_sum            'C38 H46 Mn N4 Ni2 O12'
_chemical_formula_weight         923.15
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.853(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3362(9)
_cell_length_b                   18.2471(16)
_cell_length_c                   12.2056(11)
_cell_measurement_temperature    100(2)
_cell_volume                     2105.4(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0840
_diffrn_reflns_av_sigmaI/netI    0.1182
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13927
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.8857
_exptl_absorpt_correction_T_min  0.7890
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       Block
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1477
_refine_ls_R_factor_gt           0.0829
_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)+(0.0602P)²+6.5988P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1687
_refine_ls_wR_factor_ref         0.2034
_reflns_number_gt                3007
_reflns_number_total             5198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302259t_si_002_5.cif
_cod_data_source_block           Ni2Mn
_cod_database_code               4334570
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
Ni1 Ni 0.31113(8) 0.93542(5) 0.08373(8) 0.0419(3) Uani 1 1 d .
Mn Mn 0.0000 1.0000 0.0000 0.0223(3) Uani 1 2 d S
O4 O 0.2186(4) 1.0373(2) 0.1000(3) 0.0305(9) Uani 1 1 d .
O2 O 0.2674(4) 0.9660(2) -0.0917(4) 0.0382(10) Uani 1 1 d .
O5 O 0.4099(5) 1.1035(3) 0.2021(4) 0.0583(14) Uani 1 1 d .
O1 O 0.1147(4) 0.9019(2) 0.0461(4) 0.0350(10) Uani 1 1 d .
C2 C 0.3314(9) 0.9387(4) 0.4406(7) 0.068(2) Uani 1 1 d .
H2 H 0.2757 0.9596 0.4783 0.082 Uiso 1 1 calc R
O3 O 0.0399(4) 0.9975(2) -0.1592(3) 0.0344(9) Uani 1 1 d .
C1 C 0.2902(8) 0.9421(4) 0.3184(6) 0.056(2) Uani 1 1 d .
H1 H 0.2048 0.9668 0.2714 0.067 Uiso 1 1 calc R
N1 N 0.3655(5) 0.9119(3) 0.2637(6) 0.0558(18) Uani 1 1 d .
O6 O 0.5063(4) 0.9880(3) 0.1378(4) 0.0557(14) Uani 1 1 d .
C15 C 0.0849(7) 0.8341(3) 0.0672(7) 0.050(2) Uani 1 1 d .
N2 N 0.3763(7) 0.8289(3) 0.0532(7) 0.069(2) Uani 1 1 d .
C18 C 0.2800(7) 1.0923(4) 0.1632(5) 0.0392(15) Uani 1 1 d .
C9 C 0.2481(9) 0.7872(4) -0.0237(9) 0.074(3) Uani 1 1 d .
H9A H 0.2777 0.7394 -0.0447 0.089 Uiso 1 1 calc R
H9B H 0.1981 0.8146 -0.0991 0.089 Uiso 1 1 calc R
C16 C 0.1514(6) 0.9871(3) -0.1724(6) 0.0353(14) Uani 1 1 d .
C5 C 0.4883(8) 0.8741(5) 0.3288(8) 0.067(3) Uani 1 1 d .
C14 C -0.0140(8) 0.8210(4) 0.1175(8) 0.069(3) Uani 1 1 d .
H14 H -0.0554 0.8611 0.1412 0.083 Uiso 1 1 calc R
C3 C 0.4633(10) 0.9019(4) 0.5086(7) 0.072(3) Uani 1 1 d .
H3 H 0.5010 0.9005 0.5937 0.087 Uiso 1 1 calc R
C11 C 0.1065(11) 0.7037(4) 0.0512(12) 0.117(5) Uani 1 1 d .
H11 H 0.1459 0.6629 0.0270 0.141 Uiso 1 1 calc R
C10 C 0.1465(8) 0.7736(4) 0.0358(10) 0.074(3) Uani 1 1 d .
C7 C 0.4519(9) 0.7873(5) 0.1638(10) 0.090(4) Uani 1 1 d .
H02A H 0.5014 0.7457 0.1457 0.108 Uiso 1 1 calc R
H02B H 0.3820 0.7669 0.1920 0.108 Uiso 1 1 calc R
C17 C 0.1474(7) 1.0008(5) -0.2961(6) 0.061(2) Uani 1 1 d .
H17A H 0.2409 0.9910 -0.2955 0.091 Uiso 1 1 calc R
H17B H 0.1214 1.0520 -0.3187 0.091 Uiso 1 1 calc R
H17C H 0.0773 0.9684 -0.3540 0.091 Uiso 1 1 calc R
C12 C 0.0097(12) 0.6917(5) 0.1013(13) 0.136(6) Uani 1 1 d .
H12 H -0.0146 0.6432 0.1140 0.163 Uiso 1 1 calc R
C19 C 0.1912(8) 1.1453(4) 0.1944(7) 0.063(2) Uani 1 1 d .
H19A H 0.0921 1.1297 0.1577 0.094 Uiso 1 1 calc R
H19B H 0.2003 1.1940 0.1645 0.094 Uiso 1 1 calc R
H19C H 0.2227 1.1472 0.2816 0.094 Uiso 1 1 calc R
C13 C -0.0508(10) 0.7507(5) 0.1323(12) 0.111(5) Uani 1 1 d .
H13 H -0.1193 0.7426 0.1646 0.133 Uiso 1 1 calc R
C4 C 0.5325(10) 0.8691(6) 0.4468(10) 0.084(3) Uani 1 1 d .
H4 H 0.6156 0.8417 0.4903 0.101 Uiso 1 1 calc R
C6 C 0.5565(9) 0.8317(6) 0.2615(10) 0.088(3) Uani 1 1 d .
H7A H 0.6039 0.8662 0.2269 0.106 Uiso 1 1 calc R
H7B H 0.6297 0.7989 0.3176 0.106 Uiso 1 1 calc R
C8 C 0.4693(9) 0.8367(4) -0.0128(10) 0.085(3) Uani 1 1 d .
H8A H 0.4200 0.8650 -0.0863 0.127 Uiso 1 1 calc R
H8B H 0.4927 0.7881 -0.0335 0.127 Uiso 1 1 calc R
H8C H 0.5565 0.8622 0.0379 0.127 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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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 Ni1 O2 93.93(16) . .
O1 Ni1 N1 89.72(18) . .
O2 Ni1 N1 175.5(2) . .
O1 Ni1 O6 168.92(19) . .
O2 Ni1 O6 88.96(17) . .
N1 Ni1 O6 86.95(19) . .
O1 Ni1 O4 80.52(15) . .
O2 Ni1 O4 86.73(15) . .
N1 Ni1 O4 91.2(2) . .
O6 Ni1 O4 88.98(17) . .
O1 Ni1 N2 92.5(2) . .
O2 Ni1 N2 91.0(2) . .
N1 Ni1 N2 91.6(3) . .
O6 Ni1 N2 98.1(2) . .
O4 Ni1 N2 172.5(2) . .
O1 Mn O1 180.000(1) . 3_575
O1 Mn O3 93.99(15) . 3_575
O1 Mn O3 86.01(15) 3_575 3_575
O1 Mn O3 86.01(15) . .
O1 Mn O3 93.99(15) 3_575 .
O3 Mn O3 180.0(2) 3_575 .
O1 Mn O4 76.82(15) . .
O1 Mn O4 103.18(15) 3_575 .
O3 Mn O4 91.24(14) 3_575 .
O3 Mn O4 88.76(14) . .
O1 Mn O4 103.18(15) . 3_575
O1 Mn O4 76.82(15) 3_575 3_575
O3 Mn O4 88.76(14) 3_575 3_575
O3 Mn O4 91.24(14) . 3_575
O4 Mn O4 180.0 . 3_575
C18 O4 Ni1 127.8(4) . .
C18 O4 Mn 137.0(4) . .
Ni1 O4 Mn 94.44(16) . .
C16 O2 Ni1 128.8(4) . .
C15 O1 Ni1 122.6(4) . .
C15 O1 Mn 134.3(4) . .
Ni1 O1 Mn 102.33(16) . .
C1 C2 C3 116.8(9) . .
C16 O3 Mn 130.5(4) . .
N1 C1 C2 122.5(8) . .
C1 N1 C5 120.4(7) . .
C1 N1 Ni1 118.8(4) . .
C5 N1 Ni1 120.3(6) . .
O1 C15 C10 121.0(6) . .
O1 C15 C14 120.6(6) . .
C10 C15 C14 118.4(6) . .
C7 N2 C9 108.8(6) . .
C7 N2 C8 109.1(6) . .
C9 N2 C8 108.2(7) . .
C7 N2 Ni1 113.4(6) . .
C9 N2 Ni1 108.2(4) . .
C8 N2 Ni1 109.0(4) . .
O5 C18 O4 123.9(6) . .
O5 C18 C19 118.5(6) . .
O4 C18 C19 117.6(6) . .
N2 C9 C10 113.1(8) . .
O3 C16 O2 125.7(6) . .
O3 C16 C17 116.8(6) . .
O2 C16 C17 117.5(5) . .
C4 C5 N1 119.5(10) . .
C4 C5 C6 121.9(9) . .
N1 C5 C6 118.1(8) . .
C13 C14 C15 120.3(7) . .
C4 C3 C2 117.9(8) . .
C10 C11 C12 121.1(8) . .
C11 C10 C15 119.8(7) . .
C11 C10 C9 121.3(7) . .
C15 C10 C9 118.7(6) . .
N2 C7 C6 113.6(7) . .
C13 C12 C11 119.3(8) . .
C14 C13 C12 121.0(7) . .
C5 C4 C3 122.8(10) . .
C7 C6 C5 111.8(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 1.988(4) .
Ni1 O2 2.078(4) .
Ni1 N1 2.080(6) .
Ni1 O6 2.086(4) .
Ni1 O4 2.136(4) .
Ni1 N2 2.138(6) .
Mn O1 2.095(4) .
Mn O1 2.095(4) 3_575
Mn O3 2.144(4) 3_575
Mn O3 2.144(4) .
Mn O4 2.197(4) .
Mn O4 2.197(4) 3_575
O4 C18 1.269(7) .
O2 C16 1.265(7) .
O5 C18 1.247(8) .
O1 C15 1.326(7) .
C2 C1 1.377(10) .
C2 C3 1.444(12) .
O3 C16 1.241(7) .
C1 N1 1.333(10) .
N1 C5 1.379(9) .
C15 C10 1.403(9) .
C15 C14 1.409(9) .
N2 C7 1.469(10) .
N2 C9 1.487(11) .
N2 C8 1.491(9) .
C18 C19 1.485(10) .
C9 C10 1.520(10) .
C16 C17 1.514(9) .
C5 C4 1.326(12) .
C5 C6 1.496(13) .
C14 C13 1.371(10) .
C3 C4 1.369(13) .
C11 C10 1.377(10) .
C11 C12 1.384(11) .
C7 C6 1.485(13) .
C12 C13 1.373(12) .
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
O1 Ni1 O4 C18 153.4(5) .
O2 Ni1 O4 C18 -112.0(4) .
N1 Ni1 O4 C18 63.9(5) .
O6 Ni1 O4 C18 -23.0(5) .
N2 Ni1 O4 C18 175.7(15) .
O1 Ni1 O4 Mn -17.96(15) .
O2 Ni1 O4 Mn 76.58(15) .
N1 Ni1 O4 Mn -107.47(17) .
O6 Ni1 O4 Mn 165.60(16) .
N2 Ni1 O4 Mn 4.3(16) .
O1 Mn O4 C18 -152.8(5) .
O1 Mn O4 C18 27.2(5) 3_575
O3 Mn O4 C18 -59.0(5) 3_575
O3 Mn O4 C18 121.0(5) .
O4 Mn O4 C18 -24(100) 3_575
O1 Mn O4 Ni1 17.25(14) .
O1 Mn O4 Ni1 -162.75(14) 3_575
O3 Mn O4 Ni1 111.05(15) 3_575
O3 Mn O4 Ni1 -68.95(15) .
O4 Mn O4 Ni1 146(100) 3_575
O1 Ni1 O2 C16 27.9(5) .
N1 Ni1 O2 C16 -116(3) .
O6 Ni1 O2 C16 -141.4(5) .
O4 Ni1 O2 C16 -52.4(5) .
N2 Ni1 O2 C16 120.5(5) .
O2 Ni1 O1 C15 121.8(5) .
N1 Ni1 O1 C15 -60.9(6) .
O6 Ni1 O1 C15 -133.4(9) .
O4 Ni1 O1 C15 -152.2(5) .
N2 Ni1 O1 C15 30.6(6) .
O2 Ni1 O1 Mn -66.74(19) .
N1 Ni1 O1 Mn 110.6(2) .
O6 Ni1 O1 Mn 38.1(10) .
O4 Ni1 O1 Mn 19.27(16) .
N2 Ni1 O1 Mn -157.9(2) .
O1 Mn O1 C15 3(6) 3_575
O3 Mn O1 C15 60.6(7) 3_575
O3 Mn O1 C15 -119.4(7) .
O4 Mn O1 C15 151.0(7) .
O4 Mn O1 C15 -29.0(7) 3_575
O1 Mn O1 Ni1 -167(6) 3_575
O3 Mn O1 Ni1 -109.31(18) 3_575
O3 Mn O1 Ni1 70.69(18) .
O4 Mn O1 Ni1 -18.97(16) .
O4 Mn O1 Ni1 161.03(16) 3_575
O1 Mn O3 C16 -48.1(5) .
O1 Mn O3 C16 131.9(5) 3_575
O3 Mn O3 C16 -169.6(4) 3_575
O4 Mn O3 C16 28.7(5) .
O4 Mn O3 C16 -151.3(5) 3_575
C3 C2 C1 N1 1.3(11) .
C2 C1 N1 C5 1.5(11) .
C2 C1 N1 Ni1 -169.8(5) .
O1 Ni1 N1 C1 -54.9(5) .
O2 Ni1 N1 C1 89(3) .
O6 Ni1 N1 C1 114.5(5) .
O4 Ni1 N1 C1 25.6(5) .
N2 Ni1 N1 C1 -147.4(5) .
O1 Ni1 N1 C5 133.7(6) .
O2 Ni1 N1 C5 -83(3) .
O6 Ni1 N1 C5 -56.8(6) .
O4 Ni1 N1 C5 -145.7(6) .
N2 Ni1 N1 C5 41.2(6) .
Ni1 O1 C15 C10 -45.5(10) .
Mn O1 C15 C10 146.2(6) .
Ni1 O1 C15 C14 137.0(6) .
Mn O1 C15 C14 -31.3(11) .
O1 Ni1 N2 C7 -99.4(5) .
O2 Ni1 N2 C7 166.6(5) .
N1 Ni1 N2 C7 -9.6(5) .
O6 Ni1 N2 C7 77.5(5) .
O4 Ni1 N2 C7 -121.3(15) .
O1 Ni1 N2 C9 21.5(5) .
O2 Ni1 N2 C9 -72.5(5) .
N1 Ni1 N2 C9 111.2(5) .
O6 Ni1 N2 C9 -161.6(5) .
O4 Ni1 N2 C9 -0.5(19) .
O1 Ni1 N2 C8 138.9(6) .
O2 Ni1 N2 C8 45.0(6) .
N1 Ni1 N2 C8 -131.3(6) .
O6 Ni1 N2 C8 -44.1(6) .
O4 Ni1 N2 C8 117.0(14) .
Ni1 O4 C18 O5 19.7(8) .
Mn O4 C18 O5 -172.9(4) .
Ni1 O4 C18 C19 -158.9(5) .
Mn O4 C18 C19 8.5(9) .
C7 N2 C9 C10 59.9(8) .
C8 N2 C9 C10 178.2(6) .
Ni1 N2 C9 C10 -63.8(7) .
Mn O3 C16 O2 9.4(9) .
Mn O3 C16 C17 -170.6(4) .
Ni1 O2 C16 O3 4.4(9) .
Ni1 O2 C16 C17 -175.7(4) .
C1 N1 C5 C4 -1.3(11) .
Ni1 N1 C5 C4 169.9(6) .
C1 N1 C5 C6 170.7(7) .
Ni1 N1 C5 C6 -18.0(9) .
O1 C15 C14 C13 176.1(9) .
C10 C15 C14 C13 -1.5(14) .
C1 C2 C3 C4 -4.2(11) .
C12 C11 C10 C15 -2.4(19) .
C12 C11 C10 C9 -177.5(12) .
O1 C15 C10 C11 -175.6(10) .
C14 C15 C10 C11 2.0(15) .
O1 C15 C10 C9 -0.4(14) .
C14 C15 C10 C9 177.2(9) .
N2 C9 C10 C11 -122.7(11) .
N2 C9 C10 C15 62.1(11) .
C9 N2 C7 C6 -163.4(7) .
C8 N2 C7 C6 78.8(9) .
Ni1 N2 C7 C6 -42.9(8) .
C10 C11 C12 C13 2(2) .
C15 C14 C13 C12 1.5(19) .
C11 C12 C13 C14 -2(2) .
N1 C5 C4 C3 -1.9(13) .
C6 C5 C4 C3 -173.6(8) .
C2 C3 C4 C5 4.6(13) .
N2 C7 C6 C5 83.0(9) .
C4 C5 C6 C7 125.5(9) .
N1 C5 C6 C7 -46.4(10) .
