#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317686.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_4317686
loop_
_publ_author_name
'Carole Baffert'
'Marie-Noëlle Collomb'
'Alain Deronzier'
'Jacques Pécaut'
'Julian Limburg'
'Robert H. Crabtree'
'Gary W. Brudvig'
_publ_section_title
;
 Two New Terpyridine Dimanganese Complexes: A Manganese(III,III) Complex
 with a Single Unsupported Oxo Bridge and a Manganese(III,IV) Complex with
 a Dioxo Bridge. Synthesis, Structure, and Redox Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1404
_journal_page_last               1411
_journal_paper_doi               10.1021/ic0107375
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C40 H28 Cl4 F12 Mn2 N6 O10'
_chemical_formula_weight         1232.36
_chemical_name_systematic
;
  [Mn2III,III(O)(terpy)2(CF3CO2)4].H20.2CH2Cl2
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 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                 117.838(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.528(2)
_cell_length_b                   16.6292(16)
_cell_length_c                   16.9803(17)
_cell_measurement_temperature    193(2)
_cell_volume                     4626.3(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.798
_diffrn_measured_fraction_theta_max 0.798
_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  0.0507
_diffrn_reflns_av_sigmaI/netI    0.1640
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            9003
_diffrn_reflns_theta_full        29.61
_diffrn_reflns_theta_max         29.61
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.890
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.769
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.4
_refine_diff_density_max         1.219
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.262
_refine_ls_R_factor_all          0.1735
_refine_ls_R_factor_gt           0.0869
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0880P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2519
_reflns_number_gt                2310
_reflns_number_total             5198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0107375_2.cif
_cod_data_source_block           struc_for_cis-4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4626.2(8)
_cod_database_code               4317686
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
Mn Mn 1.43221(6) -0.15038(6) 0.79483(7) 0.0197(3) Uani 1 1 d . . .
F21 F 1.1960(4) -0.2325(4) 0.8650(4) 0.081(2) Uani 1 1 d . . .
F22 F 1.2982(5) -0.1762(7) 0.9612(4) 0.159(5) Uani 1 1 d . . .
F23 F 1.2131(6) -0.1061(5) 0.8664(6) 0.137(3) Uani 1 1 d . . .
F31 F 1.3537(3) -0.4164(3) 0.8098(3) 0.0643(16) Uani 1 1 d . . .
F32 F 1.4802(3) -0.4244(3) 0.8390(4) 0.0739(18) Uani 1 1 d . . .
F33 F 1.3841(4) -0.4585(3) 0.7107(4) 0.0730(18) Uani 1 1 d . . .
O1 O 1.5000 -0.1534(4) 0.7500 0.0228(15) Uani 1 2 d S . .
O21 O 1.3586(3) -0.1451(3) 0.8487(3) 0.0238(11) Uani 1 1 d . . .
O22 O 1.2584(3) -0.2252(4) 0.7541(3) 0.0441(15) Uani 1 1 d . . .
O31 O 1.4306(3) -0.2682(3) 0.8084(3) 0.0310(12) Uani 1 1 d . . .
O32 O 1.3679(3) -0.3061(3) 0.6654(4) 0.0405(14) Uani 1 1 d . . .
N1 N 1.5373(3) -0.1349(4) 0.9309(3) 0.0255(14) Uani 1 1 d . . .
N2 N 1.4493(3) -0.0226(3) 0.8197(4) 0.0232(14) Uani 1 1 d . . .
N3 N 1.3365(3) -0.0902(4) 0.6746(3) 0.0235(14) Uani 1 1 d . . .
C1 C 1.5796(4) -0.1961(5) 0.9827(5) 0.035(2) Uani 1 1 d . . .
H1 H 1.5624 -0.2497 0.9637 0.042 Uiso 1 1 calc R . .
C2 C 1.6496(5) -0.1825(6) 1.0656(5) 0.040(2) Uani 1 1 d . . .
H2 H 1.6796 -0.2264 1.1019 0.048 Uiso 1 1 calc R . .
C3 C 1.6728(5) -0.1066(6) 1.0917(5) 0.044(2) Uani 1 1 d . . .
H3 H 1.7196 -0.0961 1.1469 0.053 Uiso 1 1 calc R . .
C4 C 1.6276(5) -0.0432(6) 1.0368(5) 0.041(2) Uani 1 1 d . . .
H4 H 1.6432 0.0108 1.0553 0.049 Uiso 1 1 calc R . .
C5 C 1.5617(4) -0.0584(4) 0.9577(4) 0.0224(16) Uani 1 1 d . . .
C6 C 1.5115(4) 0.0034(4) 0.8960(5) 0.0266(17) Uani 1 1 d . . .
C7 C 1.5265(5) 0.0853(5) 0.9118(5) 0.036(2) Uani 1 1 d . . .
H7 H 1.5709 0.1042 0.9653 0.044 Uiso 1 1 calc R . .
C8 C 1.4739(6) 0.1398(5) 0.8461(6) 0.050(2) Uani 1 1 d . . .
H8 H 1.4831 0.1960 0.8553 0.060 Uiso 1 1 calc R . .
C9 C 1.4102(5) 0.1121(5) 0.7696(6) 0.042(2) Uani 1 1 d . . .
H9 H 1.3746 0.1487 0.7256 0.051 Uiso 1 1 calc R . .
C10 C 1.3981(5) 0.0286(4) 0.7568(5) 0.0269(17) Uani 1 1 d . . .
C11 C 1.3323(4) -0.0110(4) 0.6760(4) 0.0243(17) Uani 1 1 d . . .
C12 C 1.2721(5) 0.0331(6) 0.6056(5) 0.047(2) Uani 1 1 d . . .
H12 H 1.2702 0.0901 0.6085 0.057 Uiso 1 1 calc R . .
C13 C 1.2158(5) -0.0081(5) 0.5323(5) 0.042(2) Uani 1 1 d . . .
H13 H 1.1740 0.0204 0.4841 0.050 Uiso 1 1 calc R . .
C14 C 1.2197(5) -0.0900(6) 0.5286(5) 0.040(2) Uani 1 1 d . . .
H14 H 1.1821 -0.1190 0.4777 0.048 Uiso 1 1 calc R . .
C15 C 1.2802(5) -0.1292(5) 0.6013(5) 0.0329(19) Uani 1 1 d . . .
H15 H 1.2824 -0.1862 0.6000 0.040 Uiso 1 1 calc R . .
C21 C 1.2939(4) -0.1865(4) 0.8210(5) 0.0243(16) Uani 1 1 d . . .
C22 C 1.2521(7) -0.1818(7) 0.8808(7) 0.059(3) Uani 1 1 d . . .
C31 C 1.3996(4) -0.3171(5) 0.7428(5) 0.0276(17) Uani 1 1 d . . .
C32 C 1.4040(6) -0.4041(5) 0.7759(6) 0.048(2) Uani 1 1 d . . .
C41A C 1.5034(7) -0.3831(7) 1.0373(7) 0.030(3) Uani 0.760(18) 1 d P A -1
H41A H 1.4889 -0.4408 1.0297 0.037 Uiso 0.760(18) 1 calc PR A -1
H41B H 1.5172 -0.3674 0.9897 0.037 Uiso 0.760(18) 1 calc PR A -1
C41B C 1.487(2) -0.401(2) 1.070(2) 0.030(3) Uani 0.240(18) 1 d P A -2
H41C H 1.4718 -0.4362 1.1068 0.037 Uiso 0.240(18) 1 calc PR A -2
H41D H 1.4856 -0.4341 1.0207 0.037 Uiso 0.240(18) 1 calc PR A -2
Cl2 Cl 1.4161(3) -0.3250(3) 1.0257(4) 0.181(2) Uani 1 1 d . . .
Cl1 Cl 1.5813(3) -0.3700(3) 1.1315(5) 0.203(3) Uani 1 1 d . . .
O2 O 1.4964(6) -0.3562(6) 1.2002(7) 0.035(3) Uani 0.50 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'
F F 0.0171 0.0103 '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'
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
_geom_angle_publ_flag
O1 Mn O21 178.14(18) . . ?
O1 Mn O31 94.3(2) . . ?
O21 Mn O31 86.47(19) . . ?
O1 Mn N2 92.5(2) . . ?
O21 Mn N2 86.28(19) . . ?
O31 Mn N2 164.1(2) . . ?
O1 Mn N3 92.32(17) . . ?
O21 Mn N3 88.72(19) . . ?
O31 Mn N3 120.4(2) . . ?
N2 Mn N3 73.6(2) . . ?
O1 Mn N1 89.85(14) . . ?
O21 Mn N1 88.43(19) . . ?
O31 Mn N1 92.7(2) . . ?
N2 Mn N1 73.0(2) . . ?
N3 Mn N1 146.6(2) . . ?
Mn O1 Mn 176.7(4) 2_856 . ?
C21 O21 Mn 123.0(4) . . ?
C31 O31 Mn 123.7(5) . . ?
C1 N1 C5 119.7(6) . . ?
C1 N1 Mn 123.6(5) . . ?
C5 N1 Mn 116.6(5) . . ?
C10 N2 C6 122.1(6) . . ?
C10 N2 Mn 118.7(5) . . ?
C6 N2 Mn 119.2(5) . . ?
C11 N3 C15 117.8(6) . . ?
C11 N3 Mn 117.5(5) . . ?
C15 N3 Mn 124.7(5) . . ?
N1 C1 C2 121.1(8) . . ?
C3 C2 C1 118.8(8) . . ?
C2 C3 C4 119.4(8) . . ?
C5 C4 C3 120.2(8) . . ?
N1 C5 C4 120.9(7) . . ?
N1 C5 C6 115.0(6) . . ?
C4 C5 C6 124.2(7) . . ?
N2 C6 C7 120.4(7) . . ?
N2 C6 C5 116.1(6) . . ?
C7 C6 C5 123.4(7) . . ?
C6 C7 C8 118.3(8) . . ?
C9 C8 C7 120.4(8) . . ?
C8 C9 C10 119.0(8) . . ?
N2 C10 C9 119.9(7) . . ?
N2 C10 C11 114.8(6) . . ?
C9 C10 C11 125.3(7) . . ?
N3 C11 C12 122.5(7) . . ?
N3 C11 C10 115.2(6) . . ?
C12 C11 C10 122.3(7) . . ?
C13 C12 C11 118.4(8) . . ?
C12 C13 C14 120.3(8) . . ?
C15 C14 C13 117.8(8) . . ?
N3 C15 C14 123.3(8) . . ?
O22 C21 O21 130.3(7) . . ?
O22 C21 C22 115.4(7) . . ?
O21 C21 C22 114.1(6) . . ?
F22 C22 F21 111.1(9) . . ?
F22 C22 F23 99.2(9) . . ?
F21 C22 F23 104.7(9) . . ?
F22 C22 C21 115.7(9) . . ?
F21 C22 C21 116.2(7) . . ?
F23 C22 C21 107.8(8) . . ?
O32 C31 O31 131.3(7) . . ?
O32 C31 C32 117.9(7) . . ?
O31 C31 C32 110.8(7) . . ?
F31 C32 F33 106.1(7) . . ?
F31 C32 F32 107.6(8) . . ?
F33 C32 F32 105.5(8) . . ?
F31 C32 C31 112.1(7) . . ?
F33 C32 C31 112.7(7) . . ?
F32 C32 C31 112.4(7) . . ?
Cl1 C41A Cl2 112.4(7) . . ?
Cl1 C41B Cl2 114(2) . . ?
C41B Cl2 C41A 26.0(12) . . ?
C41A Cl1 C41B 28.7(12) . . ?
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
Mn O1 1.7471(10) . ?
Mn O21 1.967(4) . ?
Mn O31 1.974(5) . ?
Mn N2 2.160(6) . ?
Mn N3 2.221(5) . ?
Mn N1 2.235(5) . ?
F21 C22 1.266(10) . ?
F22 C22 1.230(11) . ?
F23 C22 1.414(13) . ?
F31 C32 1.321(10) . ?
F32 C32 1.357(10) . ?
F33 C32 1.341(10) . ?
O1 Mn 1.7471(10) 2_856 ?
O21 C21 1.267(8) . ?
O22 C21 1.200(8) . ?
O31 C31 1.279(8) . ?
O32 C31 1.178(8) . ?
N1 C1 1.333(9) . ?
N1 C5 1.356(9) . ?
N2 C10 1.349(9) . ?
N2 C6 1.341(8) . ?
N3 C11 1.320(9) . ?
N3 C15 1.359(9) . ?
C1 C2 1.418(10) . ?
C2 C3 1.340(12) . ?
C3 C4 1.398(11) . ?
C4 C5 1.353(9) . ?
C5 C6 1.451(10) . ?
C6 C7 1.391(10) . ?
C7 C8 1.414(12) . ?
C8 C9 1.364(12) . ?
C9 C10 1.408(10) . ?
C10 C11 1.496(10) . ?
C11 C12 1.402(10) . ?
C12 C13 1.377(11) . ?
C13 C14 1.366(11) . ?
C14 C15 1.383(10) . ?
C21 C22 1.539(11) . ?
C31 C32 1.539(11) . ?
C41A Cl1 1.591(11) . ?
C41A Cl2 1.813(13) . ?
C41B Cl1 1.64(3) . ?
C41B Cl2 1.73(4) . ?
O2 O2 1.633(19) 2_857 ?
