#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:49:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179991 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/85/7028542.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_7028542
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 H44 Mn2 N10 O6, 2(N O3), 2(H2 O)'
_chemical_formula_sum            'C48 H48 Mn2 N12 O14'
_chemical_formula_weight         1126.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                95.750(5)
_cell_angle_beta                 106.408(5)
_cell_angle_gamma                103.690(6)
_cell_formula_units_Z            1
_cell_length_a                   10.5455(8)
_cell_length_b                   10.5706(9)
_cell_length_c                   11.9344(10)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.22
_cell_measurement_theta_min      2.45
_cell_volume                     1219.84(18)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1010
_diffrn_reflns_av_unetI/netI     0.1689
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9698
_diffrn_reflns_point_group_measured_fraction_full 0.930
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.343
_diffrn_reflns_theta_min         2.879
_exptl_absorpt_coefficient_mu    0.599
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_description       prism
_exptl_crystal_F_000             582
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.190
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     353
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1772
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1126P)²+1.5959P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2083
_refine_ls_wR_factor_ref         0.2520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2075
_reflns_number_total             4154
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c3dt52774c.txt
_cod_data_source_block           Compound5
_cod_database_code               7028542
#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   0.822
_shelx_estimated_absorpt_t_max   0.895
_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'
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
C2 C 0.2853(8) 0.5911(8) 1.0027(7) 0.0240(18) Uani 1 1 d . .
C3 C 0.3078(8) 0.6684(8) 1.1128(7) 0.031(2) Uani 1 1 d . .
C4 C 0.2066(8) 0.7202(8) 1.1365(7) 0.029(2) Uani 1 1 d . .
H4 H 0.2223 0.7702 1.2123 0.035 Uiso 1 1 calc R U
C5 C 0.0828(8) 0.6974(9) 1.0475(8) 0.035(2) Uani 1 1 d . .
H5 H 0.0131 0.7325 1.0629 0.042 Uiso 1 1 calc R U
C6 C 0.0581(8) 0.6262(8) 0.9385(7) 0.031(2) Uani 1 1 d . .
H6 H -0.0269 0.6154 0.8783 0.037 Uiso 1 1 calc R U
C7 C 0.1570(8) 0.5680(8) 0.9133(7) 0.0283(19) Uani 1 1 d . .
C8 C 0.1177(8) 0.4902(8) 0.7977(7) 0.031(2) Uani 1 1 d . .
H8 H 0.0324 0.4894 0.7426 0.037 Uiso 1 1 calc R U
C9 C 0.1942(8) 0.2666(8) 0.6115(7) 0.029(2) Uani 1 1 d . .
C10 C 0.1282(8) 0.1874(8) 0.4910(7) 0.030(2) Uani 1 1 d . .
C11 C 0.0415(8) 0.2331(9) 0.4023(7) 0.036(2) Uani 1 1 d . .
H11 H 0.0270 0.3172 0.4199 0.043 Uiso 1 1 calc R U
C12 C -0.0238(9) 0.1584(10) 0.2895(8) 0.041(2) Uani 1 1 d . .
H12 H -0.0822 0.1906 0.2298 0.049 Uiso 1 1 calc R U
C13 C -0.0014(8) 0.0327(10) 0.2649(7) 0.040(2) Uani 1 1 d . .
H13 H -0.0477 -0.0214 0.1889 0.048 Uiso 1 1 calc R U
C14 C 0.0858(9) -0.0107(9) 0.3496(8) 0.037(2) Uani 1 1 d . .
H14 H 0.1025 -0.0933 0.3302 0.045 Uiso 1 1 calc R U
C15 C 0.1528(8) 0.0636(9) 0.4661(7) 0.031(2) Uani 1 1 d . .
C21 C 0.3607(9) 0.1151(9) 0.9246(9) 0.045(3) Uani 1 1 d . .
H21 H 0.4138 0.1019 0.8744 0.054 Uiso 1 1 calc R U
C22 C 0.3140(11) 0.0131(10) 0.9781(9) 0.054(3) Uani 1 1 d . .
H22 H 0.3350 -0.0686 0.9653 0.064 Uiso 1 1 calc R U
C23 C 0.2375(10) 0.0305(10) 1.0495(10) 0.056(3) Uani 1 1 d . .
H23 H 0.2058 -0.0388 1.0883 0.067 Uiso 1 1 calc R U
C24 C 0.2056(10) 0.1493(10) 1.0657(9) 0.050(3) Uani 1 1 d . .
H24 H 0.1505 0.1630 1.1140 0.060 Uiso 1 1 calc R U
C25 C 0.2569(8) 0.2467(9) 1.0090(7) 0.034(2) Uani 1 1 d . .
H25 H 0.2357 0.3287 1.0197 0.040 Uiso 1 1 calc R U
C31 C 0.5557(10) 0.5727(12) 0.6928(9) 0.059(3) Uani 1 1 d . .
H31 H 0.5830 0.4943 0.6807 0.071 Uiso 1 1 calc R U
C32 C 0.6020(11) 0.6773(13) 0.6391(10) 0.066(3) Uani 1 1 d . .
H32 H 0.6608 0.6710 0.5927 0.079 Uiso 1 1 calc R U
C33 C 0.5598(10) 0.7925(11) 0.6551(9) 0.055(3) Uani 1 1 d . .
H33 H 0.5907 0.8669 0.6214 0.066 Uiso 1 1 calc R U
C34 C 0.4733(10) 0.7937(11) 0.7204(9) 0.053(3) Uani 1 1 d . .
H34 H 0.4393 0.8683 0.7298 0.063 Uiso 1 1 calc R U
C35 C 0.4353(9) 0.6888(9) 0.7723(8) 0.043(2) Uani 1 1 d . .
H35 H 0.3774 0.6935 0.8198 0.052 Uiso 1 1 calc R U
N1 N 0.3348(7) 0.2330(7) 0.9398(6) 0.0367(18) Uani 1 1 d . .
N2 N 0.4768(7) 0.5767(8) 0.7590(6) 0.0384(19) Uani 1 1 d . .
N3 N 0.2408(7) 0.0143(7) 0.5470(6) 0.0352(18) Uani 1 1 d . .
N10 N 0.7788(9) 0.3609(11) 0.5516(8) 0.059(3) Uani 1 1 d . .
N11 N 0.1895(7) 0.4211(7) 0.7629(6) 0.0295(16) Uani 1 1 d . .
N12 N 0.1282(7) 0.3491(7) 0.6486(6) 0.0318(18) Uani 1 1 d . .
O1 O 0.3870(5) 0.5414(5) 0.9893(4) 0.0284(13) Uani 1 1 d . .
O2 O 0.3054(6) 0.2605(6) 0.6801(5) 0.0415(16) Uani 1 1 d . .
O3 O 0.4338(5) 0.6890(6) 1.1929(5) 0.0381(16) Uani 1 1 d . .
H3 H 0.4581 0.7435 1.2682 0.046 Uiso 1 1 calc R U
O10 O 0.5387(7) 0.1303(8) 0.6312(6) 0.0542(19) Uani 1 1 d D .
O11 O 0.7695(11) 0.2475(8) 0.5567(7) 0.089(3) Uani 1 1 d . .
O12 O 0.8853(9) 0.4189(10) 0.5245(7) 0.084(3) Uani 1 1 d . .
O13 O 0.7107(13) 0.4240(12) 0.5722(13) 0.158(6) Uani 1 1 d . .
Mn1 Mn 0.41295(12) 0.40826(13) 0.85493(11) 0.0278(4) Uani 1 1 d . .
H3A H 0.2848 0.0603 0.6192 0.042 Uiso 1 1 d . U
H3B H 0.2524 -0.0636 0.5273 0.042 Uiso 1 1 d . U
H12A H 0.051(9) 0.344(9) 0.608(8) 0.042 Uiso 1 1 d . U
H10B H 0.602(5) 0.186(7) 0.604(6) 0.042 Uiso 1 1 d D U
H10A H 0.451(3) 0.095(7) 0.582(5) 0.042 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 C2 C3 117.5(7) . .
O1 C2 C7 123.8(7) . .
C3 C2 C7 118.7(6) . .
O3 C3 C4 123.0(7) . .
O3 C3 C2 115.4(7) . .
C4 C3 C2 121.6(7) . .
C5 C4 C3 118.6(8) . .
C5 C4 H4 120.7 . .
C3 C4 H4 120.7 . .
C6 C5 C4 121.7(7) . .
C6 C5 H5 119.1 . .
C4 C5 H5 119.1 . .
C5 C6 C7 120.9(7) . .
C5 C6 H6 119.5 . .
C7 C6 H6 119.5 . .
C6 C7 C2 118.3(7) . .
C6 C7 C8 116.2(7) . .
C2 C7 C8 125.4(7) . .
N11 C8 C7 124.7(7) . .
N11 C8 H8 117.6 . .
C7 C8 H8 117.6 . .
O2 C9 N12 119.0(7) . .
O2 C9 C10 123.8(7) . .
N12 C9 C10 117.2(6) . .
C11 C10 C15 120.1(8) . .
C11 C10 C9 120.8(7) . .
C15 C10 C9 119.1(7) . .
C12 C11 C10 121.4(8) . .
C12 C11 H11 119.3 . .
C10 C11 H11 119.3 . .
C11 C12 C13 118.5(8) . .
C11 C12 H12 120.7 . .
C13 C12 H12 120.7 . .
C14 C13 C12 120.4(8) . .
C14 C13 H13 119.8 . .
C12 C13 H13 119.8 . .
C13 C14 C15 122.0(8) . .
C13 C14 H14 119.0 . .
C15 C14 H14 119.0 . .
N3 C15 C10 123.6(7) . .
N3 C15 C14 118.9(7) . .
C10 C15 C14 117.5(7) . .
N1 C21 C22 123.0(9) . .
N1 C21 H21 118.5 . .
C22 C21 H21 118.5 . .
C23 C22 C21 119.1(9) . .
C23 C22 H22 120.5 . .
C21 C22 H22 120.5 . .
C22 C23 C24 119.9(10) . .
C22 C23 H23 120.1 . .
C24 C23 H23 120.1 . .
C25 C24 C23 117.3(9) . .
C25 C24 H24 121.3 . .
C23 C24 H24 121.3 . .
N1 C25 C24 124.0(8) . .
N1 C25 H25 118.0 . .
C24 C25 H25 118.0 . .
N2 C31 C32 123.4(10) . .
N2 C31 H31 118.3 . .
C32 C31 H31 118.3 . .
C31 C32 C33 118.5(10) . .
C31 C32 H32 120.8 . .
C33 C32 H32 120.8 . .
C34 C33 C32 117.7(10) . .
C34 C33 H33 121.2 . .
C32 C33 H33 121.2 . .
C35 C34 C33 120.3(10) . .
C35 C34 H34 119.9 . .
C33 C34 H34 119.9 . .
C34 C35 N2 122.8(9) . .
C34 C35 H35 118.6 . .
N2 C35 H35 118.6 . .
C25 N1 C21 116.7(8) . .
C25 N1 Mn1 118.8(5) . .
C21 N1 Mn1 124.5(6) . .
C31 N2 C35 117.3(8) . .
C31 N2 Mn1 122.5(7) . .
C35 N2 Mn1 120.2(6) . .
C15 N3 H3A 120.0 . .
C15 N3 H3B 120.2 . .
H3A N3 H3B 120.00 . .
O13 N10 O11 129.1(12) . .
O13 N10 O12 117.7(12) . .
O11 N10 O12 113.2(9) . .
C8 N11 N12 114.6(6) . .
C8 N11 Mn1 130.9(6) . .
N12 N11 Mn1 114.4(4) . .
C9 N12 N11 116.8(6) . .
C9 N12 H12A 118(6) . .
N11 N12 H12A 124(6) . .
C2 O1 Mn1 136.0(5) . .
C2 O1 Mn1 118.2(4) . 2_667
Mn1 O1 Mn1 105.63(19) . 2_667
C9 O2 Mn1 120.6(5) . .
C3 O3 Mn1 119.3(5) . 2_667
C3 O3 H3 120.3 . .
Mn1 O3 H3 120.3 2_667 .
H10B O10 H10A 118(5) . .
O1 Mn1 N2 91.7(2) . .
O1 Mn1 O3 143.7(2) . 2_667
N2 Mn1 O3 89.9(2) . 2_667
O1 Mn1 O1 74.4(2) . 2_667
N2 Mn1 O1 97.4(2) . 2_667
O3 Mn1 O1 69.50(18) 2_667 2_667
O1 Mn1 O2 145.6(2) . .
N2 Mn1 O2 92.3(3) . .
O3 Mn1 O2 70.41(19) 2_667 .
O1 Mn1 O2 138.64(18) 2_667 .
O1 Mn1 N1 89.9(2) . .
N2 Mn1 N1 175.9(3) . .
O3 Mn1 N1 91.0(2) 2_667 .
O1 Mn1 N1 86.7(2) 2_667 .
O2 Mn1 N1 84.3(3) . .
O1 Mn1 N11 78.7(2) . .
N2 Mn1 N11 84.2(2) . .
O3 Mn1 N11 137.4(2) 2_667 .
O1 Mn1 N11 153.1(2) 2_667 .
O2 Mn1 N11 67.8(2) . .
N1 Mn1 N11 92.4(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C2 O1 1.340(8) .
C2 C3 1.404(11) .
C2 C7 1.416(11) .
C3 O3 1.353(9) .
C3 C4 1.390(10) .
C4 C5 1.380(11) .
C4 H4 0.9500 .
C5 C6 1.359(11) .
C5 H5 0.9500 .
C6 C7 1.415(10) .
C6 H6 0.9500 .
C7 C8 1.427(11) .
C8 N11 1.288(9) .
C8 H8 0.9500 .
C9 O2 1.247(9) .
C9 N12 1.352(10) .
C9 C10 1.473(11) .
C10 C11 1.398(11) .
C10 C15 1.412(11) .
C11 C12 1.385(12) .
C11 H11 0.9500 .
C12 C13 1.420(12) .
C12 H12 0.9500 .
C13 C14 1.359(11) .
C13 H13 0.9500 .
C14 C15 1.419(11) .
C14 H14 0.9500 .
C15 N3 1.374(9) .
C21 N1 1.343(10) .
C21 C22 1.370(14) .
C21 H21 0.9500 .
C22 C23 1.356(14) .
C22 H22 0.9500 .
C23 C24 1.384(13) .
C23 H23 0.9500 .
C24 C25 1.375(12) .
C24 H24 0.9500 .
C25 N1 1.339(10) .
C25 H25 0.9500 .
C31 N2 1.304(11) .
C31 C32 1.391(15) .
C31 H31 0.9500 .
C32 C33 1.405(15) .
C32 H32 0.9500 .
C33 C34 1.358(13) .
C33 H33 0.9500 .
C34 C35 1.356(13) .
C34 H34 0.9500 .
C35 N2 1.367(11) .
C35 H35 0.9500 .
N1 Mn1 2.295(7) .
N2 Mn1 2.282(7) .
N3 H3A 0.882 .
N3 H3B 0.879 .
N10 O13 1.146(10) .
N10 O11 1.189(12) .
N10 O12 1.288(12) .
N11 N12 1.385(9) .
N11 Mn1 2.345(6) .
N12 H12A 0.80(8) .
O1 Mn1 2.146(5) .
O1 Mn1 2.290(5) 2_667
O2 Mn1 2.291(6) .
O3 Mn1 2.277(5) 2_667
O3 H3 0.9500 .
O10 H10B 0.93(2) .
O10 H10A 0.91(2) .
Mn1 O3 2.277(5) 2_667
Mn1 O1 2.290(5) 2_667
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
N3 H3A O2 0.882 2.110 2.735(9) 128.0 .
N3 H3B O11 0.879 2.030 2.880(10) 163.7(5) 2_656
N12 H12A O12 0.80(8) 2.13(8) 2.876(10) 155(9) 1_455
O10 H10B O11 0.93(2) 1.99(4) 2.876(13) 158(7) .
O10 H10B N10 0.93(2) 2.56(3) 3.487(13) 172(7) .
O10 H10B O13 0.93(2) 2.62(5) 3.453(15) 149(7) .
O10 H10A N3 0.91(2) 2.08(4) 2.920(10) 153(6) .
O3 H3 O10 0.95 1.69 2.594(9) 157.8 2_667
