#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:49:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179991 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/85/7028541.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_7028541
loop_
_publ_author_name
'Sutradhar, Manas'
'Martins, Luísa M D R S'
'Guedes da Silva, M Fátima C'
'Alegria, Elisabete C. B. A.'
'Liu, Cai-Ming'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Dinuclear Mn(ii,ii) complexes: magnetic properties and microwave assisted
 oxidation of alcohols.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3966
_journal_page_last               3977
_journal_paper_doi               10.1039/c3dt52774c
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C48 H42 Mn2 N8 O6, 2(N O3), H2 O'
_chemical_formula_sum            'C48 H44 Mn2 N10 O13'
_chemical_formula_weight         1078.81
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.2330(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.8357(4)
_cell_length_b                   17.3807(5)
_cell_length_c                   23.5331(6)
_cell_measurement_reflns_used    8555
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.32
_cell_measurement_theta_min      2.34
_cell_volume                     5166.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.847
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX-II PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.847
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17872
_diffrn_reflns_point_group_measured_fraction_full 0.847
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         24.362
_diffrn_reflns_theta_min         2.291
_exptl_absorpt_coefficient_mu    0.560
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         3953
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0887P)²+11.1031P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3062
_reflns_number_total             3953
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3dt52774c.txt
_cod_data_source_block           Compound4
_cod_database_code               7028541
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.887
_shelxl_version_number           2013-4
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
C1 C 0.6896(3) 0.3887(2) 0.53263(15) 0.0394(8) Uani 1 1 d . . .
C2 C 0.6915(3) 0.4465(2) 0.48830(16) 0.0407(8) Uani 1 1 d . . .
C3 C 0.6547(3) 0.5190(2) 0.49373(19) 0.0534(10) Uani 1 1 d . . .
H3 H 0.6551 0.5552 0.4646 0.064 Uiso 1 1 calc R U .
C4 C 0.6145(4) 0.5389(2) 0.5459(2) 0.0634(12) Uani 1 1 d . . .
H4 H 0.5892 0.5885 0.5497 0.076 Uiso 1 1 calc R U .
C5 C 0.6128(3) 0.4859(2) 0.59065(19) 0.0566(11) Uani 1 1 d . . .
H5 H 0.5877 0.5007 0.6237 0.068 Uiso 1 1 calc R U .
C6 C 0.6489(3) 0.4102(2) 0.58557(16) 0.0430(9) Uani 1 1 d . . .
C7 C 0.6397(3) 0.3599(2) 0.63550(17) 0.0484(10) Uani 1 1 d . . .
H7 H 0.6156 0.3820 0.6668 0.058 Uiso 1 1 calc R U .
C8 C 0.6645(3) 0.1753(2) 0.69472(16) 0.0476(9) Uani 1 1 d . . .
C9 C 0.6491(3) 0.1346(3) 0.75190(17) 0.0513(10) Uani 1 1 d . . .
C10 C 0.6352(4) 0.1727(3) 0.80507(19) 0.0672(12) Uani 1 1 d . . .
H10 H 0.6351 0.2262 0.8059 0.081 Uiso 1 1 calc R U .
C11 C 0.6218(4) 0.1321(4) 0.8561(2) 0.0815(16) Uani 1 1 d . . .
H11 H 0.6118 0.1585 0.8891 0.098 Uiso 1 1 calc R U .
C12 C 0.6241(4) 0.0530(4) 0.8552(2) 0.0885(17) Uani 1 1 d . . .
H12 H 0.6165 0.0249 0.8878 0.106 Uiso 1 1 calc R U .
C13 C 0.6383(4) 0.0146(3) 0.8034(2) 0.0850(16) Uani 1 1 d . . .
H13 H 0.6397 -0.0389 0.8030 0.102 Uiso 1 1 calc R U .
C14 C 0.6506(4) 0.0556(3) 0.7520(2) 0.0677(12) Uani 1 1 d . . .
H14 H 0.6594 0.0288 0.7190 0.081 Uiso 1 1 calc R U .
C21 C 0.9573(4) 0.1713(3) 0.6474(2) 0.0738(14) Uani 1 1 d . . .
H21 H 0.9339 0.1209 0.6413 0.089 Uiso 1 1 calc R U .
C22 C 1.0570(4) 0.1839(4) 0.6814(3) 0.0887(17) Uani 1 1 d . . .
H22 H 1.0996 0.1427 0.6962 0.106 Uiso 1 1 calc R U .
C23 C 1.0900(4) 0.2573(4) 0.6921(2) 0.0839(16) Uani 1 1 d . . .
H23 H 1.1551 0.2674 0.7153 0.101 Uiso 1 1 calc R U .
C24 C 1.0263(4) 0.3167(3) 0.6684(2) 0.0756(14) Uani 1 1 d . . .
H24 H 1.0475 0.3675 0.6749 0.091 Uiso 1 1 calc R U .
C25 C 0.9295(3) 0.2992(3) 0.63437(19) 0.0609(12) Uani 1 1 d . . .
H25 H 0.8870 0.3398 0.6184 0.073 Uiso 1 1 calc R U .
C31 C 0.4873(3) 0.2473(3) 0.5095(2) 0.0604(11) Uani 1 1 d . . .
H31 H 0.5105 0.2965 0.5211 0.072 Uiso 1 1 calc R U .
C32 C 0.3860(4) 0.2389(3) 0.4782(2) 0.0695(13) Uani 1 1 d . . .
H32 H 0.3430 0.2818 0.4689 0.083 Uiso 1 1 calc R U .
C33 C 0.3499(4) 0.1678(3) 0.4610(2) 0.0751(14) Uani 1 1 d . . .
H33 H 0.2822 0.1608 0.4398 0.090 Uiso 1 1 calc R U .
C34 C 0.4163(4) 0.1065(3) 0.4761(3) 0.0901(18) Uani 1 1 d . . .
H34 H 0.3943 0.0568 0.4654 0.108 Uiso 1 1 calc R U .
C35 C 0.5169(4) 0.1195(3) 0.5076(2) 0.0703(13) Uani 1 1 d . . .
H35 H 0.5609 0.0774 0.5178 0.084 Uiso 1 1 calc R U .
N2 N 0.8938(3) 0.22805(19) 0.62318(14) 0.0509(8) Uani 1 1 d . . .
N3 N 0.5536(2) 0.18856(18) 0.52403(14) 0.0487(8) Uani 1 1 d . . .
N11 N 0.6626(2) 0.28889(18) 0.63828(13) 0.0456(8) Uani 1 1 d D . .
N12 N 0.6452(3) 0.2509(2) 0.69070(13) 0.0521(8) Uani 1 1 d D . .
H12A H 0.6236 0.2758 0.7179 0.062 Uiso 1 1 calc R U .
O1 O 0.72352(19) 0.31914(14) 0.52185(10) 0.0423(6) Uani 1 1 d . . .
O2 O 0.6950(3) 0.14131(17) 0.65319(13) 0.0681(9) Uani 1 1 d . . .
O3 O 0.7330(2) 0.42184(15) 0.43787(12) 0.0568(7) Uani 1 1 d . . .
H3A H 0.7431 0.4565 0.4093 0.068 Uiso 1 1 calc R U .
Mn1 Mn 0.72689(4) 0.20822(3) 0.56859(2) 0.0408(2) Uani 1 1 d . . .
O42 O 0.7356(4) 0.9638(2) 0.63667(19) 0.1122(15) Uani 1 1 d . . .
O20W O 1.0000 0.8350(4) 0.7500 0.120(2) Uani 1 2 d DS T P
N40 N 0.8080(6) 0.9274(4) 0.6706(2) 0.1145(19) Uani 1 1 d . . .
O41 O 0.8880(6) 0.9317(8) 0.6641(4) 0.335(9) Uani 1 1 d . . .
O40 O 0.7853(5) 0.8848(3) 0.7096(3) 0.160(2) Uani 1 1 d . . .
H20A H 0.943(7) 0.859(6) 0.722(4) 0.240 Uiso 1 1 d D U .
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'
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 C1 C2 116.5(3) . .
O1 C1 C6 124.7(3) . .
C2 C1 C6 118.9(3) . .
C3 C2 C1 121.6(3) . .
C3 C2 O3 122.4(3) . .
C1 C2 O3 116.1(3) . .
C2 C3 C4 118.7(4) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
C5 C4 C3 122.2(4) . .
C5 C4 H4 118.9 . .
C3 C4 H4 118.9 . .
C4 C5 C6 120.1(4) . .
C4 C5 H5 120.0 . .
C6 C5 H5 120.0 . .
C5 C6 C1 118.6(3) . .
C5 C6 C7 114.1(3) . .
C1 C6 C7 127.2(3) . .
N11 C7 C6 124.3(4) . .
N11 C7 H7 117.9 . .
C6 C7 H7 117.9 . .
O2 C8 N12 118.9(3) . .
O2 C8 C9 124.0(4) . .
N12 C8 C9 117.1(3) . .
C14 C9 C10 117.2(4) . .
C14 C9 C8 116.7(4) . .
C10 C9 C8 126.0(4) . .
C11 C10 C9 123.4(5) . .
C11 C10 H10 118.3 . .
C9 C10 H10 118.3 . .
C12 C11 C10 118.2(5) . .
C12 C11 H11 120.9 . .
C10 C11 H11 120.9 . .
C11 C12 C13 119.2(4) . .
C11 C12 H12 120.4 . .
C13 C12 H12 120.4 . .
C12 C13 C14 122.4(5) . .
C12 C13 H13 118.8 . .
C14 C13 H13 118.8 . .
C9 C14 C13 119.6(5) . .
C9 C14 H14 120.2 . .
C13 C14 H14 120.2 . .
N2 C21 C22 123.6(5) . .
N2 C21 H21 118.2 . .
C22 C21 H21 118.2 . .
C23 C22 C21 118.5(5) . .
C23 C22 H22 120.7 . .
C21 C22 H22 120.7 . .
C22 C23 C24 119.2(5) . .
C22 C23 H23 120.4 . .
C24 C23 H23 120.4 . .
C23 C24 C25 118.6(5) . .
C23 C24 H24 120.7 . .
C25 C24 H24 120.7 . .
N2 C25 C24 124.1(4) . .
N2 C25 H25 118.0 . .
C24 C25 H25 118.0 . .
N3 C31 C32 123.5(4) . .
N3 C31 H31 118.2 . .
C32 C31 H31 118.2 . .
C33 C32 C31 119.6(5) . .
C33 C32 H32 120.2 . .
C31 C32 H32 120.2 . .
C32 C33 C34 117.8(4) . .
C32 C33 H33 121.1 . .
C34 C33 H33 121.1 . .
C33 C34 C35 119.2(5) . .
C33 C34 H34 120.4 . .
C35 C34 H34 120.4 . .
N3 C35 C34 123.6(4) . .
N3 C35 H35 118.2 . .
C34 C35 H35 118.2 . .
C25 N2 C21 116.0(4) . .
C25 N2 Mn1 120.0(3) . .
C21 N2 Mn1 123.9(3) . .
C35 N3 C31 116.3(4) . .
C35 N3 Mn1 122.1(3) . .
C31 N3 Mn1 121.5(3) . .
C7 N11 N12 114.7(3) . .
C7 N11 Mn1 129.4(3) . .
N12 N11 Mn1 115.9(2) . .
C8 N12 N11 117.0(3) . .
C8 N12 H12A 121.5 . .
N11 N12 H12A 121.5 . .
C1 O1 Mn1 132.6(2) . .
C1 O1 Mn1 120.3(2) . 7_656
Mn1 O1 Mn1 106.61(10) . 7_656
C8 O2 Mn1 122.5(3) . .
C2 O3 Mn1 117.3(2) . 7_656
C2 O3 H3A 121.4 . .
Mn1 O3 H3A 121.4 7_656 .
O1 Mn1 N3 88.34(10) . .
O1 Mn1 N2 94.60(11) . .
N3 Mn1 N2 173.49(12) . .
O1 Mn1 O3 142.82(9) . 7_656
N3 Mn1 O3 91.90(11) . 7_656
N2 Mn1 O3 89.26(11) . 7_656
O1 Mn1 O1 73.39(10) . 7_656
N3 Mn1 O1 87.33(10) . 7_656
N2 Mn1 O1 99.07(10) . 7_656
O3 Mn1 O1 69.49(9) 7_656 7_656
O1 Mn1 O2 147.27(10) . .
N3 Mn1 O2 90.73(12) . .
N2 Mn1 O2 83.65(12) . .
O3 Mn1 O2 69.91(10) 7_656 .
O1 Mn1 O2 139.26(10) 7_656 .
O1 Mn1 N11 81.54(10) . .
N3 Mn1 N11 88.65(11) . .
N2 Mn1 N11 86.05(11) . .
O3 Mn1 N11 135.64(10) 7_656 .
O1 Mn1 N11 154.71(10) 7_656 .
O2 Mn1 N11 65.72(10) . .
O41 N40 O40 120.1(8) . .
O41 N40 O42 119.2(8) . .
O40 N40 O42 120.7(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.325(4) .
C1 C2 1.452(5) .
C1 C6 1.482(5) .
C2 C3 1.361(5) .
C2 O3 1.449(4) .
C3 C4 1.455(6) .
C3 H3 0.9300 .
C4 C5 1.404(6) .
C4 H4 0.9300 .
C5 C6 1.406(5) .
C5 H5 0.9300 .
C6 C7 1.486(5) .
C7 N11 1.268(5) .
C7 H7 0.9300 .
C8 O2 1.262(5) .
C8 N12 1.338(5) .
C8 C9 1.563(5) .
C9 C14 1.373(6) .
C9 C10 1.454(6) .
C10 C11 1.430(7) .
C10 H10 0.9300 .
C11 C12 1.376(8) .
C11 H11 0.9300 .
C12 C13 1.429(8) .
C12 H12 0.9300 .
C13 C14 1.437(7) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C21 N2 1.340(6) .
C21 C22 1.400(7) .
C21 H21 0.9300 .
C22 C23 1.355(8) .
C22 H22 0.9300 .
C23 C24 1.372(7) .
C23 H23 0.9300 .
C24 C25 1.386(6) .
C24 H24 0.9300 .
C25 N2 1.329(5) .
C25 H25 0.9300 .
C31 N3 1.333(5) .
C31 C32 1.384(6) .
C31 H31 0.9300 .
C32 C33 1.356(7) .
C32 H32 0.9300 .
C33 C34 1.372(7) .
C33 H33 0.9300 .
C34 C35 1.388(7) .
C34 H34 0.9300 .
C35 N3 1.321(5) .
C35 H35 0.9300 .
N2 Mn1 2.320(3) .
N3 Mn1 2.310(3) .
N11 N12 1.451(4) .
N11 Mn1 2.412(3) .
N12 H12A 0.8600 .
O1 Mn1 2.216(2) .
O1 Mn1 2.375(2) 7_656
O2 Mn1 2.402(3) .
O3 Mn1 2.329(3) 7_656
O3 H3A 0.9300 .
Mn1 O3 2.330(3) 7_656
Mn1 O1 2.375(2) 7_656
O42 N40 1.280(7) .
O20W H20A 0.99(2) .
N40 O41 1.067(8) .
N40 O40 1.253(7) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N12 H12A O20W 0.86 2.14 2.913(5) 149.8 3_445
O20W H20A O41 0.99(2) 1.90(5) 2.819(9) 154(10) .
O20W H20A O40 0.99(2) 2.05(8) 2.884(7) 141(10) .
O20W H20A N40 0.99(2) 2.27(3) 3.242(8) 170(10) .
O3 H3A O42 0.93 1.81 2.728(5) 170.2 7_666
