#------------------------------------------------------------------------------
#$Date: 2021-04-16 11:46:56 +0300 (Fri, 16 Apr 2021) $
#$Revision: 264242 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/33/4313325.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_4313325
loop_
_publ_author_name
'Yilma Gultneh'
'Teshome B. Yisgedu'
'Yohannes T. Tesema'
'Ray J. Butcher'
_publ_section_title
;
 Dioxo-Bridged Dinuclear Manganese(III) and -(IV) Complexes of Pyridyl
 Donor Tripod Ligands: Combined Effects of Steric Substitution and Chelate
 Ring Size Variations on Structural, Spectroscopic, and Electrochemical
 Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1857
_journal_page_last               1867
_journal_paper_doi               10.1021/ic020131w
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H48 Cl2 Mn2 N8 O10'
_chemical_formula_weight         1005.66
_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                65.628(6)
_cell_angle_beta                 80.426(7)
_cell_angle_gamma                86.505(7)
_cell_formula_units_Z            1
_cell_length_a                   9.0081(7)
_cell_length_b                   11.5356(10)
_cell_length_c                   11.8101(10)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.19
_cell_measurement_theta_min      1.96
_cell_volume                     1102.26(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω 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  0.0145
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5236
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.10
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  0.8673
_exptl_absorpt_correction_T_min  0.5658
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.99
_exptl_crystal_size_min          0.76
_refine_diff_density_max         0.435
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4928
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0386
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+0.5104P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                4551
_reflns_number_total             4928
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020131w_1.cif
_cod_data_source_block           ty189c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

2021-04-13
Formula fixed to be consistent with given Z value
                 miguel
;
_cod_original_formula_sum            'C21 H24 Cl Mn N4 O5'
_cod_original_formula_weight         502.83
_cod_original_cell_volume        1102.26(16)
_cod_database_code               4313325
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
Mn Mn 0.53242(3) 0.53915(2) 0.58648(2) 0.02694(10) Uani 1 1 d . . .
Cl Cl 0.92981(6) 0.82192(5) 0.84352(6) 0.05079(15) Uani 1 1 d . . .
O O 0.36712(13) 0.48613(12) 0.54923(11) 0.0311(3) Uani 1 1 d . . .
O1 O 0.7913(3) 0.8850(2) 0.8307(4) 0.1132(10) Uani 1 1 d . . .
O2 O 0.8992(3) 0.6906(2) 0.9204(2) 0.0857(7) Uani 1 1 d . . .
O3 O 1.0009(4) 0.8266(3) 0.7262(3) 0.1295(12) Uani 1 1 d . . .
O4 O 1.0270(3) 0.8760(3) 0.8889(3) 0.1134(10) Uani 1 1 d . . .
N N 0.73889(16) 0.59588(15) 0.61394(14) 0.0315(3) Uani 1 1 d . . .
N1A N 0.54039(19) 0.76751(15) 0.48106(15) 0.0374(3) Uani 1 1 d . . .
N1B N 0.63090(18) 0.35013(15) 0.73535(14) 0.0340(3) Uani 1 1 d . . .
N1C N 0.44618(17) 0.57711(14) 0.74957(13) 0.0297(3) Uani 1 1 d . . .
C1A C 0.2740(3) 0.8078(2) 0.4708(2) 0.0549(6) Uani 1 1 d . . .
H1AA H 0.2710 0.7208 0.4816 0.074(9) Uiso 1 1 calc R . .
H1AB H 0.2178 0.8594 0.4054 0.117(14) Uiso 1 1 calc R . .
H1AC H 0.2307 0.8140 0.5481 0.080(10) Uiso 1 1 calc R . .
C2A C 0.4333(3) 0.8533(2) 0.4358(2) 0.0452(5) Uani 1 1 d . . .
C3A C 0.4714(4) 0.9804(2) 0.3593(3) 0.0624(7) Uani 1 1 d . . .
H3AA H 0.3971 1.0381 0.3255 0.065(8) Uiso 1 1 calc R . .
C4A C 0.6179(4) 1.0202(2) 0.3340(3) 0.0713(8) Uani 1 1 d . . .
H4AA H 0.6436 1.1050 0.2836 0.079(9) Uiso 1 1 calc R . .
C5A C 0.7269(3) 0.9337(2) 0.3838(2) 0.0599(6) Uani 1 1 d . . .
H5AA H 0.8267 0.9591 0.3700 0.092(11) Uiso 1 1 calc R . .
C6A C 0.6842(3) 0.8080(2) 0.45477(19) 0.0424(5) Uani 1 1 d . . .
C7A C 0.8000(2) 0.7070(2) 0.49823(19) 0.0430(5) Uani 1 1 d . . .
H7AA H 0.8367 0.6788 0.4319 0.040(6) Uiso 1 1 calc R . .
H7AB H 0.8845 0.7429 0.5145 0.052(7) Uiso 1 1 calc R . .
C1B C 0.4004(3) 0.2242(2) 0.8240(2) 0.0532(6) Uani 1 1 d . . .
H1BA H 0.3660 0.2869 0.7502 0.066(8) Uiso 1 1 calc R . .
H1BB H 0.3524 0.2372 0.8967 0.092(11) Uiso 1 1 calc R . .
H1BC H 0.3757 0.1407 0.8330 0.107(13) Uiso 1 1 calc R . .
C2B C 0.5666(3) 0.2363(2) 0.81171(18) 0.0410(4) Uani 1 1 d . . .
C3B C 0.6540(3) 0.1348(2) 0.8771(2) 0.0562(6) Uani 1 1 d . . .
H3BA H 0.6098 0.0552 0.9253 0.081(10) Uiso 1 1 calc R . .
C4B C 0.8049(3) 0.1513(2) 0.8710(3) 0.0618(7) Uani 1 1 d . . .
H4BA H 0.8629 0.0839 0.9166 0.081(10) Uiso 1 1 calc R . .
C5B C 0.8697(3) 0.2691(2) 0.7962(2) 0.0515(5) Uani 1 1 d . . .
H5BA H 0.9712 0.2838 0.7924 0.064(8) Uiso 1 1 calc R . .
C6B C 0.7793(2) 0.3649(2) 0.72718(18) 0.0374(4) Uani 1 1 d . . .
C7B C 0.8457(2) 0.4894(2) 0.63036(19) 0.0388(4) Uani 1 1 d . . .
H7BA H 0.9357 0.5076 0.6555 0.056(7) Uiso 1 1 calc R . .
H7BB H 0.8749 0.4826 0.5505 0.050(7) Uiso 1 1 calc R . .
C1C C 0.1794(2) 0.5199(3) 0.7729(2) 0.0471(5) Uani 1 1 d . . .
H1CA H 0.2158 0.5104 0.6961 0.092(11) Uiso 1 1 calc R . .
H1CB H 0.0975 0.5790 0.7602 0.099(12) Uiso 1 1 calc R . .
H1CC H 0.1450 0.4390 0.8378 0.098(12) Uiso 1 1 calc R . .
C2C C 0.3033(2) 0.56879(18) 0.81113(16) 0.0328(4) Uani 1 1 d . . .
C3C C 0.2687(2) 0.6071(2) 0.90963(18) 0.0404(4) Uani 1 1 d . . .
H3CA H 0.1704 0.5998 0.9516 0.054(7) Uiso 1 1 calc R . .
C4C C 0.3790(3) 0.6556(2) 0.94488(19) 0.0444(5) Uani 1 1 d . . .
H4CA H 0.3558 0.6830 1.0095 0.063(8) Uiso 1 1 calc R . .
C5C C 0.5249(2) 0.6633(2) 0.88373(19) 0.0401(4) Uani 1 1 d . . .
H5CA H 0.6018 0.6951 0.9068 0.045(6) Uiso 1 1 calc R . .
C6C C 0.5543(2) 0.62276(16) 0.78734(16) 0.0302(3) Uani 1 1 d . . .
C7C C 0.7157(2) 0.6275(2) 0.72576(19) 0.0406(4) Uani 1 1 d . . .
H7CA H 0.7555 0.7123 0.7004 0.059(8) Uiso 1 1 calc R . .
H7CB H 0.7735 0.5686 0.7877 0.063(8) 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'
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
O Mn O 84.56(6) . 2_666 ?
O Mn N 173.69(5) . . ?
O Mn N 89.17(5) 2_666 . ?
O Mn N1C 104.01(6) . . ?
O Mn N1C 171.43(5) 2_666 . ?
N Mn N1C 82.26(6) . . ?
O Mn N1B 105.14(6) . . ?
O Mn N1B 93.36(6) 2_666 . ?
N Mn N1B 74.57(6) . . ?
N1C Mn N1B 84.33(5) . . ?
O Mn N1A 106.85(6) . . ?
O Mn N1A 94.73(6) 2_666 . ?
N Mn N1A 74.21(6) . . ?
N1C Mn N1A 83.03(6) . . ?
N1B Mn N1A 147.58(6) . . ?
O Mn Mn 42.31(4) . 2_666 ?
O Mn Mn 42.25(4) 2_666 2_666 ?
N Mn Mn 131.41(4) . 2_666 ?
N1C Mn Mn 146.32(4) . 2_666 ?
N1B Mn Mn 102.48(4) . 2_666 ?
N1A Mn Mn 104.57(4) . 2_666 ?
O4 Cl O1 112.23(18) . . ?
O4 Cl O3 108.1(2) . . ?
O1 Cl O3 109.9(2) . . ?
O4 Cl O2 113.31(18) . . ?
O1 Cl O2 107.68(16) . . ?
O3 Cl O2 105.33(18) . . ?
Mn O Mn 95.44(6) . 2_666 ?
C7B N C7A 108.07(15) . . ?
C7B N C7C 111.04(15) . . ?
C7A N C7C 111.08(16) . . ?
C7B N Mn 107.51(11) . . ?
C7A N Mn 108.41(12) . . ?
C7C N Mn 110.61(11) . . ?
C6A N1A C2A 118.54(18) . . ?
C6A N1A Mn 109.29(13) . . ?
C2A N1A Mn 131.74(14) . . ?
C6B N1B C2B 118.90(17) . . ?
C6B N1B Mn 109.32(12) . . ?
C2B N1B Mn 131.48(14) . . ?
C6C N1C C2C 118.11(15) . . ?
C6C N1C Mn 111.90(11) . . ?
C2C N1C Mn 129.86(12) . . ?
N1A C2A C3A 120.7(2) . . ?
N1A C2A C1A 117.7(2) . . ?
C3A C2A C1A 121.6(2) . . ?
C4A C3A C2A 120.1(2) . . ?
C3A C4A C5A 119.4(2) . . ?
C4A C5A C6A 118.3(3) . . ?
N1A C6A C5A 123.0(2) . . ?
N1A C6A C7A 116.22(17) . . ?
C5A C6A C7A 120.6(2) . . ?
N C7A C6A 112.18(16) . . ?
N1B C2B C3B 120.3(2) . . ?
N1B C2B C1B 117.85(19) . . ?
C3B C2B C1B 121.8(2) . . ?
C4B C3B C2B 120.5(2) . . ?
C3B C4B C5B 119.1(2) . . ?
C4B C5B C6B 118.0(2) . . ?
N1B C6B C5B 123.0(2) . . ?
N1B C6B C7B 115.85(17) . . ?
C5B C6B C7B 121.00(19) . . ?
N C7B C6B 112.22(15) . . ?
N1C C2C C3C 121.02(17) . . ?
N1C C2C C1C 120.42(16) . . ?
C3C C2C C1C 118.55(17) . . ?
C4C C3C C2C 120.05(18) . . ?
C3C C4C C5C 119.42(17) . . ?
C4C C5C C6C 118.46(19) . . ?
N1C C6C C5C 122.93(17) . . ?
N1C C6C C7C 119.80(15) . . ?
C5C C6C C7C 117.25(17) . . ?
N C7C C6C 114.99(15) . . ?
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 O 1.8264(12) . ?
Mn O 1.8285(12) 2_666 ?
Mn N 2.1253(15) . ?
Mn N1C 2.1592(14) . ?
Mn N1B 2.3982(16) . ?
Mn N1A 2.4044(17) . ?
Mn Mn 2.7042(5) 2_666 ?
Cl O4 1.393(2) . ?
Cl O1 1.404(2) . ?
Cl O3 1.408(3) . ?
Cl O2 1.424(2) . ?
O Mn 1.8285(12) 2_666 ?
N C7B 1.481(2) . ?
N C7A 1.485(2) . ?
N C7C 1.489(2) . ?
N1A C6A 1.346(3) . ?
N1A C2A 1.347(3) . ?
N1B C6B 1.340(2) . ?
N1B C2B 1.347(3) . ?
N1C C6C 1.351(2) . ?
N1C C2C 1.356(2) . ?
C1A C2A 1.490(4) . ?
C2A C3A 1.396(3) . ?
C3A C4A 1.368(4) . ?
C4A C5A 1.377(4) . ?
C5A C6A 1.383(3) . ?
C6A C7A 1.498(3) . ?
C1B C2B 1.489(3) . ?
C2B C3B 1.389(3) . ?
C3B C4B 1.370(4) . ?
C4B C5B 1.379(4) . ?
C5B C6B 1.385(3) . ?
C6B C7B 1.500(3) . ?
C1C C2C 1.491(3) . ?
C2C C3C 1.390(2) . ?
C3C C4C 1.367(3) . ?
C4C C5C 1.379(3) . ?
C5C C6C 1.382(2) . ?
C6C C7C 1.507(3) . ?
