#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:07:06 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193793 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/17/7041717.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_7041717
loop_
_publ_author_name
'Escriche-Tur, Luis'
'Font-Bardia, Mercè'
'Albela, Belén'
'Corbella, Montserrat'
_publ_section_title
;
 Determination of ZFS parameters from the EPR spectra of mono-, di- and
 trinuclear Mn(II) complexes: impact of magnetic coupling.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2699
_journal_page_last               2714
_journal_paper_doi               10.1039/c6dt04012h
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C64 H46 Mn2 N8 O6, 2(Cl O4)'
_chemical_formula_sum            'C64 H46 Cl2 Mn2 N8 O14'
_chemical_formula_weight         1331.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2016-12-14 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.929(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8275(19)
_cell_length_b                   19.625(2)
_cell_length_c                   9.5828(12)
_cell_measurement_reflns_used    9819
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.54
_cell_measurement_theta_min      2.65
_cell_volume                     2778.2(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_source         'high brilliance Incoatec Microfocus Source '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1343
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            40561
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.583
_diffrn_reflns_theta_min         2.650
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       plaque
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.763
_refine_diff_density_min         -1.696
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.173
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     239
_refine_ls_number_reflns         4379
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0247P)²+23.6954P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4007
_reflns_number_total             4379
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt04012h2.cif
_cod_data_source_block           Compound_7
_cod_depositor_comments
'Adding full bibliography for 7041716--7041723.cif.'
_cod_database_code               7041717
_shelx_shelxl_version_number     2016/6
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.500000 0.20255(7) 0.500000 0.0336(3) Uani 1 2 d DS T P . .
O4 O 0.4601(3) 0.2654(2) 0.4540(6) 0.0317(12) Uani 0.5 1 d D . P A 1
O6 O 0.4128(3) 0.1922(4) 0.5417(6) 0.0415(15) Uani 0.5 1 d D . P A 1
O5 O 0.4361(4) 0.1468(3) 0.4739(8) 0.0512(19) Uani 0.5 1 d D . P A -1
O7 O 0.4896(4) 0.2127(4) 0.3467(4) 0.0479(17) Uani 0.5 1 d D . P A -1
Mn1 Mn 0.000000 0.08775(3) 0.000000 0.01064(14) Uani 1 2 d S T P . .
O1 O -0.06844(19) 0.000000 -0.1010(3) 0.0130(5) Uani 1 2 d S T P . .
O2 O -0.0919(2) 0.000000 -0.3356(3) 0.0186(6) Uani 1 2 d S T P . .
O3 O -0.4988(2) 0.000000 -0.1757(4) 0.0257(7) Uani 1 2 d S T P . .
N1 N 0.10087(16) 0.10668(12) -0.1596(3) 0.0138(4) Uani 1 1 d . . . . .
N2 N 0.11244(17) 0.15131(12) 0.1096(3) 0.0147(5) Uani 1 1 d . . . . .
C1 C 0.0939(2) 0.08731(16) -0.2929(3) 0.0175(5) Uani 1 1 d . . . . .
H1 H 0.039177 0.069074 -0.330344 0.021 Uiso 1 1 calc R U . . .
C2 C 0.1649(2) 0.09300(16) -0.3799(3) 0.0195(6) Uani 1 1 d . . . . .
H2 H 0.156451 0.080400 -0.473669 0.023 Uiso 1 1 calc R U . . .
C3 C 0.2473(2) 0.11751(16) -0.3245(3) 0.0197(6) Uani 1 1 d . . . . .
H3 H 0.295384 0.121223 -0.380201 0.024 Uiso 1 1 calc R U . . .
C4 C 0.2581(2) 0.13695(15) -0.1824(3) 0.0162(5) Uani 1 1 d . . . . .
C5 C 0.3430(2) 0.16078(17) -0.1155(4) 0.0206(6) Uani 1 1 d . . . . .
H5 H 0.393513 0.163670 -0.166522 0.025 Uiso 1 1 calc R U . . .
C6 C 0.3496(2) 0.17891(17) 0.0208(4) 0.0209(6) Uani 1 1 d . . . . .
H6 H 0.405245 0.193046 0.063069 0.025 Uiso 1 1 calc R U . . .
C7 C 0.2731(2) 0.17695(15) 0.1020(3) 0.0174(6) Uani 1 1 d . . . . .
C8 C 0.2765(2) 0.19685(16) 0.2432(3) 0.0205(6) Uani 1 1 d . . . . .
H8 H 0.330875 0.211188 0.289451 0.025 Uiso 1 1 calc R U . . .
C9 C 0.1994(2) 0.19509(16) 0.3127(3) 0.0213(6) Uani 1 1 d . . . . .
H9 H 0.201047 0.208942 0.405729 0.026 Uiso 1 1 calc R U . . .
C10 C 0.1181(2) 0.17219(15) 0.2422(3) 0.0180(6) Uani 1 1 d . . . . .
H10 H 0.066157 0.171595 0.290097 0.022 Uiso 1 1 calc R U . . .
C11 C 0.18829(19) 0.15404(14) 0.0389(3) 0.0137(5) Uani 1 1 d . . . . .
C12 C 0.18174(19) 0.13244(14) -0.1046(3) 0.0128(5) Uani 1 1 d . . . . .
C13 C -0.1212(3) 0.000000 -0.2182(4) 0.0124(7) Uani 1 2 d S T P . .
C14 C -0.2209(3) 0.000000 -0.2063(4) 0.0124(7) Uani 1 2 d S T P . .
C15 C -0.2578(3) 0.000000 -0.0773(4) 0.0131(7) Uani 1 2 d S T P . .
H15 H -0.219387 0.000000 0.004720 0.016 Uiso 1 2 calc R U P . .
C16 C -0.3510(3) 0.000000 -0.0692(4) 0.0163(8) Uani 1 2 d S T P . .
H16 H -0.374879 0.000000 0.017435 0.020 Uiso 1 2 calc R U P . .
C17 C -0.4086(3) 0.000000 -0.1934(5) 0.0178(8) Uani 1 2 d S T P . .
C18 C -0.3733(3) 0.000000 -0.3224(5) 0.0214(9) Uani 1 2 d S T P . .
H18 H -0.411595 0.000000 -0.404523 0.026 Uiso 1 2 calc R U P . .
C19 C -0.2798(3) 0.000000 -0.3280(4) 0.0178(8) Uani 1 2 d S T P . .
H19 H -0.256102 0.000000 -0.414696 0.021 Uiso 1 2 calc R U P . .
C20 C -0.5593(3) 0.000000 -0.2991(5) 0.0262(10) Uani 1 2 d S T P . .
H20A H -0.620591 0.000000 -0.273734 0.039 Uiso 1 2 calc R U P . .
H20B H -0.549161 0.039941 -0.353380 0.039 Uiso 0.5 1 calc R U P . .
H20C H -0.549161 -0.039941 -0.353380 0.039 Uiso 0.5 1 calc R U 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'
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'
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'
H H 0.0000 0.0000 '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
O6 Cl1 O6 163.3(6) . 2_656
O6 Cl1 O4 114.0(4) . 2_656
O6 Cl1 O4 81.0(4) 2_656 2_656
O6 Cl1 O4 81.0(4) . .
O6 Cl1 O4 114.0(4) 2_656 .
O4 Cl1 O4 59.7(4) 2_656 .
O6 Cl1 O5 48.4(4) . .
O6 Cl1 O5 116.5(5) 2_656 .
O4 Cl1 O5 162.4(4) 2_656 .
O4 Cl1 O5 110.5(3) . .
O6 Cl1 O5 116.5(5) . 2_656
O6 Cl1 O5 48.4(4) 2_656 2_656
O4 Cl1 O5 110.5(3) 2_656 2_656
O4 Cl1 O5 162.4(4) . 2_656
O5 Cl1 O5 82.5(6) . 2_656
O6 Cl1 O7 75.9(4) . 2_656
O6 Cl1 O7 106.4(3) 2_656 2_656
O4 Cl1 O7 64.5(3) 2_656 2_656
O4 Cl1 O7 101.3(4) . 2_656
O5 Cl1 O7 106.4(3) . 2_656
O5 Cl1 O7 85.4(4) 2_656 2_656
O6 Cl1 O7 106.4(3) . .
O6 Cl1 O7 75.9(4) 2_656 .
O4 Cl1 O7 101.3(4) 2_656 .
O4 Cl1 O7 64.5(3) . .
O5 Cl1 O7 85.4(4) . .
O5 Cl1 O7 106.4(3) 2_656 .
O7 Cl1 O7 164.5(6) 2_656 .
O4 O4 Cl1 60.2(2) 2_656 .
O4 O4 O7 98.3(4) 2_656 .
Cl1 O4 O7 59.5(2) . .
O5 O6 Cl1 68.2(3) . .
O6 O5 Cl1 63.4(2) . .
Cl1 O7 O4 56.0(2) . .
O1 Mn1 O1 75.80(12) . 5
O1 Mn1 N1 98.00(10) . .
O1 Mn1 N1 96.90(10) 5 .
O1 Mn1 N1 96.90(10) . 2
O1 Mn1 N1 98.00(10) 5 2
N1 Mn1 N1 161.08(13) . 2
O1 Mn1 N2 159.25(9) . .
O1 Mn1 N2 86.17(9) 5 .
N1 Mn1 N2 73.74(9) . .
N1 Mn1 N2 95.69(9) 2 .
O1 Mn1 N2 86.17(9) . 2
O1 Mn1 N2 159.25(9) 5 2
N1 Mn1 N2 95.69(9) . 2
N1 Mn1 N2 73.74(9) 2 2
N2 Mn1 N2 113.23(13) . 2
C13 O1 Mn1 126.84(7) . .
C13 O1 Mn1 126.84(7) . 5
Mn1 O1 Mn1 104.20(12) . 5
C17 O3 C20 116.9(4) . .
C1 N1 C12 118.1(3) . .
C1 N1 Mn1 127.0(2) . .
C12 N1 Mn1 114.23(18) . .
C10 N2 C11 118.4(3) . .
C10 N2 Mn1 126.6(2) . .
C11 N2 Mn1 113.36(18) . .
N1 C1 C2 123.3(3) . .
N1 C1 H1 118.4 . .
C2 C1 H1 118.4 . .
C3 C2 C1 119.0(3) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C2 C3 C4 119.4(3) . .
C2 C3 H3 120.3 . .
C4 C3 H3 120.3 . .
C3 C4 C12 117.6(3) . .
C3 C4 C5 122.6(3) . .
C12 C4 C5 119.7(3) . .
C6 C5 C4 120.2(3) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 121.7(3) . .
C5 C6 H6 119.1 . .
C7 C6 H6 119.1 . .
C8 C7 C11 117.0(3) . .
C8 C7 C6 123.6(3) . .
C11 C7 C6 119.4(3) . .
C9 C8 C7 119.9(3) . .
C9 C8 H8 120.0 . .
C7 C8 H8 120.0 . .
C8 C9 C10 119.4(3) . .
C8 C9 H9 120.3 . .
C10 C9 H9 120.3 . .
N2 C10 C9 122.6(3) . .
N2 C10 H10 118.7 . .
C9 C10 H10 118.7 . .
N2 C11 C7 122.6(3) . .
N2 C11 C12 118.3(3) . .
C7 C11 C12 119.1(3) . .
N1 C12 C4 122.5(3) . .
N1 C12 C11 117.7(2) . .
C4 C12 C11 119.8(3) . .
O2 C13 O1 123.2(4) . .
O2 C13 C14 119.7(3) . .
O1 C13 C14 117.1(4) . .
C15 C14 C19 118.4(4) . .
C15 C14 C13 122.3(3) . .
C19 C14 C13 119.3(4) . .
C16 C15 C14 121.1(4) . .
C16 C15 H15 119.4 . .
C14 C15 H15 119.4 . .
C15 C16 C17 119.2(4) . .
C15 C16 H16 120.4 . .
C17 C16 H16 120.4 . .
O3 C17 C18 124.2(4) . .
O3 C17 C16 115.3(4) . .
C18 C17 C16 120.5(4) . .
C17 C18 C19 119.3(4) . .
C17 C18 H18 120.4 . .
C19 C18 H18 120.4 . .
C18 C19 C14 121.5(4) . .
C18 C19 H19 119.2 . .
C14 C19 H19 119.2 . .
O3 C20 H20A 109.5 . .
O3 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
O3 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl1 O6 1.401(4) .
Cl1 O6 1.401(4) 2_656
Cl1 O4 1.421(4) 2_656
Cl1 O4 1.421(3) .
Cl1 O5 1.454(4) .
Cl1 O5 1.454(4) 2_656
Cl1 O7 1.477(4) 2_656
Cl1 O7 1.477(4) .
O4 O4 1.414(10) 2_656
O4 O7 1.547(8) .
O6 O5 1.171(9) .
Mn1 O1 2.1824(18) .
Mn1 O1 2.1824(18) 5
Mn1 N1 2.260(2) .
Mn1 N1 2.260(2) 2
Mn1 N2 2.267(2) .
Mn1 N2 2.267(2) 2
O1 C13 1.312(5) .
O2 C13 1.240(5) .
O3 C17 1.362(5) .
O3 C20 1.422(6) .
N1 C1 1.328(4) .
N1 C12 1.365(4) .
N2 C10 1.331(4) .
N2 C11 1.363(4) .
C1 C2 1.403(4) .
C1 H1 0.9300 .
C2 C3 1.376(5) .
C2 H2 0.9300 .
C3 C4 1.410(4) .
C3 H3 0.9300 .
C4 C12 1.410(4) .
C4 C5 1.441(4) .
C5 C6 1.350(5) .
C5 H5 0.9300 .
C6 C7 1.429(4) .
C6 H6 0.9300 .
C7 C8 1.405(4) .
C7 C11 1.421(4) .
C8 C9 1.371(5) .
C8 H8 0.9300 .
C9 C10 1.405(4) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.434(4) .
C13 C14 1.492(5) .
C14 C15 1.394(6) .
C14 C19 1.395(5) .
C15 C16 1.392(6) .
C15 H15 0.9300 .
C16 C17 1.404(6) .
C16 H16 0.9300 .
C17 C18 1.384(6) .
C18 C19 1.391(6) .
C18 H18 0.9300 .
C19 H19 0.9300 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
