#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:48:46 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229182 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/67/7046762.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_7046762
loop_
_publ_author_name
'Gupta, Vijay'
'Mandal, Sanjay K.'
_publ_section_title
;
 Coordination driven self-assembly of [2 + 2 + 2] molecular squares:
 synthesis, crystal structures, catalytic and luminescence properties.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9742
_journal_page_last               9754
_journal_paper_doi               10.1039/c8dt01367e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C60 H62 Mn2 N6 O12'
_chemical_formula_sum            'C60 H62 Mn2 N6 O12'
_chemical_formula_weight         1169.03
_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
_atom_sites_solution_primary     dual
_audit_update_record
;
2018-06-01 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                73.892(4)
_cell_angle_beta                 87.146(4)
_cell_angle_gamma                63.605(4)
_cell_formula_units_Z            1
_cell_length_a                   9.061(3)
_cell_length_b                   9.991(3)
_cell_length_c                   17.405(5)
_cell_measurement_reflns_used    853
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.6657
_cell_measurement_theta_min      2.3479
_cell_volume                     1351.0(7)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_collection       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19882
_diffrn_reflns_theta_full        25.12
_diffrn_reflns_theta_max         25.12
_diffrn_reflns_theta_min         1.22
_diffrn_source                   'Sealed tube'
_diffrn_source_type              'Fine Focus'
_exptl_absorpt_coefficient_mu    0.539
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6934
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangle
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.441
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0340
_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)+(0.0344P)²+1.3955P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0908
_reflns_number_gt                4142
_reflns_number_total             4793
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01367e2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7046761--7046765.cif.'
_cod_database_code               7046762
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_posn
_atom_site_occupancy
Mn Mn1 0.43380(4) 0.21330(4) 0.18583(2) 0.01225(11) Uani d . . 1
O O1 0.45750(19) 0.36193(19) 0.24537(10) 0.0184(4) Uani d . . 1
O O2 0.6316(2) 0.44037(19) 0.17260(10) 0.0220(4) Uani d . . 1
O O3 1.16123(19) 0.01857(19) 0.83199(10) 0.0197(4) Uani d . . 1
O O4 1.35160(19) -0.02679(19) 0.74269(10) 0.0197(4) Uani d . . 1
O O5 0.7479(2) 0.52798(18) 0.50933(9) 0.0183(4) Uani d . . 1
O O6 0.59292(19) 0.26364(18) 0.09194(9) 0.0163(3) Uani d . . 1
H H6A 0.6891 0.1819 0.0963 0.024 Uiso d U R 1
H H6B 0.6201 0.3335 0.0993 0.024 Uiso d U R 1
N N1 0.2129(2) 0.4270(2) 0.11221(11) 0.0157(4) Uani d . . 1
N N2 0.1907(2) 0.2047(2) 0.24213(11) 0.0143(4) Uani d . . 1
N N3 0.3966(2) 0.0426(2) 0.13854(11) 0.0147(4) Uani d . . 1
C C1 0.5640(3) 0.4149(3) 0.23585(14) 0.0153(5) Uani d . . 1
C C2 0.6119(3) 0.4453(3) 0.30846(14) 0.0143(5) Uani d . . 1
C C3 0.6129(3) 0.3535(3) 0.38515(14) 0.0170(5) Uani d . . 1
H H3 0.5796 0.2736 0.3914 0.02 Uiso calc U R 1
C C4 0.6616(3) 0.3766(3) 0.45226(14) 0.0185(5) Uani d . . 1
H H4 0.6636 0.3122 0.5043 0.022 Uiso calc U R 1
C C5 0.7074(3) 0.4947(3) 0.44279(13) 0.0143(5) Uani d . . 1
C C6 0.7044(3) 0.5896(3) 0.36793(14) 0.0170(5) Uani d . . 1
H H6 0.734 0.6717 0.3622 0.02 Uiso calc U R 1
C C7 0.6572(3) 0.5637(3) 0.30053(14) 0.0162(5) Uani d . . 1
H H7 0.6561 0.6278 0.2486 0.019 Uiso calc U R 1
C C8 0.8575(3) 0.4029(3) 0.56983(14) 0.0152(5) Uani d . . 1
C C9 0.8256(3) 0.4038(3) 0.64825(14) 0.0156(5) Uani d . . 1
H H9 0.7287 0.4848 0.6595 0.019 Uiso calc U R 1
C C10 0.9371(3) 0.2846(3) 0.71052(14) 0.0149(5) Uani d . . 1
H H10 0.9149 0.2837 0.7645 0.018 Uiso calc U R 1
C C11 1.0807(3) 0.1667(3) 0.69469(14) 0.0140(5) Uani d . . 1
C C12 1.1104(3) 0.1686(3) 0.61506(14) 0.0168(5) Uani d . . 1
H H12 1.2079 0.0887 0.6036 0.02 Uiso calc U R 1
C C13 0.9994(3) 0.2857(3) 0.55252(14) 0.0184(5) Uani d . . 1
H H13 1.0199 0.2858 0.4985 0.022 Uiso calc U R 1
C C14 1.2060(3) 0.0435(3) 0.76205(14) 0.0148(5) Uani d . . 1
C C15 0.2199(3) 0.5239(3) 0.04227(14) 0.0182(5) Uani d . . 1
H H15 0.3149 0.4881 0.0135 0.022 Uiso calc U R 1
C C16 0.0956(3) 0.6726(3) 0.01065(15) 0.0213(5) Uani d . . 1
H H16 0.1057 0.7385 -0.0383 0.026 Uiso calc U R 1
C C17 -0.0440(3) 0.7237(3) 0.05168(16) 0.0281(6) Uani d . . 1
H H17 -0.1317 0.8257 0.0315 0.034 Uiso calc U R 1
C C18 -0.0538(3) 0.6234(3) 0.12299(15) 0.0249(6) Uani d . . 1
H H18 -0.1497 0.6552 0.1516 0.03 Uiso calc U R 1
C C19 0.0775(3) 0.4769(3) 0.15196(14) 0.0159(5) Uani d . . 1
C C20 0.0745(3) 0.3706(3) 0.23267(14) 0.0161(5) Uani d . . 1
H H20A 0.1034 0.4041 0.2758 0.019 Uiso calc U R 1
H H20B -0.039 0.381 0.2389 0.019 Uiso calc U R 1
C C21 0.1236(3) 0.1503(3) 0.18721(14) 0.0171(5) Uani d . . 1
H H21A 0.0502 0.242 0.1436 0.02 Uiso calc U R 1
H H21B 0.0552 0.1026 0.2175 0.02 Uiso calc U R 1
C C22 0.2533(3) 0.0339(3) 0.15012(13) 0.0148(5) Uani d . . 1
C C23 0.2212(3) -0.0738(3) 0.12683(14) 0.0182(5) Uani d . . 1
H H23 0.1178 -0.0761 0.1347 0.022 Uiso calc U R 1
C C24 0.3419(3) -0.1770(3) 0.09211(14) 0.0209(5) Uani d . . 1
H H24 0.3228 -0.2518 0.076 0.025 Uiso calc U R 1
C C25 0.4914(3) -0.1705(3) 0.08101(14) 0.0189(5) Uani d . . 1
H H25 0.5765 -0.2406 0.0574 0.023 Uiso calc U R 1
C C26 0.5136(3) -0.0599(3) 0.10505(13) 0.0166(5) Uani d . . 1
H H26 0.6162 -0.0557 0.0977 0.02 Uiso calc U R 1
C C27 0.2169(3) 0.1060(3) 0.32915(14) 0.0166(5) Uani d . . 1
C C28 0.3136(3) 0.1507(3) 0.37886(14) 0.0205(5) Uani d . . 1
H H28A 0.4175 0.1389 0.3552 0.031 Uiso calc U R 1
H H28B 0.3376 0.0825 0.434 0.031 Uiso calc U R 1
H H28C 0.2474 0.2593 0.3791 0.031 Uiso calc U R 1
C C29 0.0528(3) 0.1269(3) 0.36536(15) 0.0226(5) Uani d . . 1
H H29A -0.0101 0.2347 0.3675 0.034 Uiso calc U R 1
H H29B 0.0753 0.0558 0.4198 0.034 Uiso calc U R 1
H H29C -0.0115 0.1036 0.332 0.034 Uiso calc U R 1
C C30 0.3224(3) -0.0650(3) 0.33245(15) 0.0225(5) Uani d . . 1
H H30A 0.259 -0.1001 0.306 0.034 Uiso calc U R 1
H H30B 0.3535 -0.1285 0.3886 0.034 Uiso calc U R 1
H H30C 0.4225 -0.0762 0.3049 0.034 Uiso calc U R 1
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Mn1 O4 . 2_756 88.27(7)
O1 Mn1 O6 . . 91.33(6)
O4 Mn1 O6 2_756 . 89.72(6)
O1 Mn1 N3 . . 172.13(6)
O4 Mn1 N3 2_756 . 89.52(7)
O6 Mn1 N3 . . 96.22(6)
O1 Mn1 N1 . . 86.84(7)
O4 Mn1 N1 2_756 . 174.78(7)
O6 Mn1 N1 . . 88.56(7)
N3 Mn1 N1 . . 95.57(7)
O1 Mn1 N2 . . 98.75(6)
O4 Mn1 N2 2_756 . 109.86(7)
O6 Mn1 N2 . . 158.10(6)
N3 Mn1 N2 . . 74.92(7)
N1 Mn1 N2 . . 72.75(7)
C1 O1 Mn1 . . 127.39(14)
C14 O4 Mn1 . 2_756 129.96(15)
C8 O5 C5 . . 117.13(17)
Mn1 O6 H6A . . 111.2
Mn1 O6 H6B . . 110.6
H6A O6 H6B . . 102.9
C19 N1 C15 . . 118.4(2)
C19 N1 Mn1 . . 114.65(15)
C15 N1 Mn1 . . 124.93(15)
C20 N2 C21 . . 107.29(17)
C20 N2 C27 . . 111.75(17)
C21 N2 C27 . . 112.52(17)
C20 N2 Mn1 . . 103.95(13)
C21 N2 Mn1 . . 105.54(13)
C27 N2 Mn1 . . 115.08(13)
C22 N3 C26 . . 118.0(2)
C22 N3 Mn1 . . 117.59(15)
C26 N3 Mn1 . . 124.17(15)
O2 C1 O1 . . 125.6(2)
O2 C1 C2 . . 118.7(2)
O1 C1 C2 . . 115.7(2)
C7 C2 C3 . . 118.7(2)
C7 C2 C1 . . 120.9(2)
C3 C2 C1 . . 120.3(2)
C4 C3 C2 . . 121.1(2)
C4 C3 H3 . . 119.5
C2 C3 H3 . . 119.5
C3 C4 C5 . . 119.2(2)
C3 C4 H4 . . 120.4
C5 C4 H4 . . 120.4
C6 C5 C4 . . 121.2(2)
C6 C5 O5 . . 117.7(2)
C4 C5 O5 . . 120.9(2)
C5 C6 C7 . . 119.1(2)
C5 C6 H6 . . 120.5
C7 C6 H6 . . 120.5
C2 C7 C6 . . 120.8(2)
C2 C7 H7 . . 119.6
C6 C7 H7 . . 119.6
C9 C8 O5 . . 117.5(2)
C9 C8 C13 . . 121.0(2)
O5 C8 C13 . . 121.4(2)
C8 C9 C10 . . 119.2(2)
C8 C9 H9 . . 120.4
C10 C9 H9 . . 120.4
C9 C10 C11 . . 120.9(2)
C9 C10 H10 . . 119.6
C11 C10 H10 . . 119.6
C10 C11 C12 . . 118.9(2)
C10 C11 C14 . . 120.7(2)
C12 C11 C14 . . 120.4(2)
C13 C12 C11 . . 120.8(2)
C13 C12 H12 . . 119.6
C11 C12 H12 . . 119.6
C12 C13 C8 . . 119.2(2)
C12 C13 H13 . . 120.4
C8 C13 H13 . . 120.4
O3 C14 O4 . . 125.1(2)
O3 C14 C11 . . 119.0(2)
O4 C14 C11 . . 115.9(2)
N1 C15 C16 . . 123.0(2)
N1 C15 H15 . . 118.5
C16 C15 H15 . . 118.5
C15 C16 C17 . . 118.6(2)
C15 C16 H16 . . 120.7
C17 C16 H16 . . 120.7
C16 C17 C18 . . 118.9(2)
C16 C17 H17 . . 120.6
C18 C17 H17 . . 120.6
C19 C18 C17 . . 119.3(2)
C19 C18 H18 . . 120.3
C17 C18 H18 . . 120.3
N1 C19 C18 . . 121.9(2)
N1 C19 C20 . . 118.0(2)
C18 C19 C20 . . 120.1(2)
N2 C20 C19 . . 112.65(18)
N2 C20 H20A . . 109.1
C19 C20 H20A . . 109.1
N2 C20 H20B . . 109.1
C19 C20 H20B . . 109.1
H20A C20 H20B . . 107.8
N2 C21 C22 . . 114.56(18)
N2 C21 H21A . . 108.6
C22 C21 H21A . . 108.6
N2 C21 H21B . . 108.6
C22 C21 H21B . . 108.6
H21A C21 H21B . . 107.6
N3 C22 C23 . . 122.2(2)
N3 C22 C21 . . 117.21(19)
C23 C22 C21 . . 120.6(2)
C24 C23 C22 . . 119.0(2)
C24 C23 H23 . . 120.5
C22 C23 H23 . . 120.5
C23 C24 C25 . . 119.2(2)
C23 C24 H24 . . 120.4
C25 C24 H24 . . 120.4
C26 C25 C24 . . 118.4(2)
C26 C25 H25 . . 120.8
C24 C25 H25 . . 120.8
N3 C26 C25 . . 123.1(2)
N3 C26 H26 . . 118.4
C25 C26 H26 . . 118.4
N2 C27 C30 . . 108.49(18)
N2 C27 C29 . . 112.14(19)
C30 C27 C29 . . 109.81(19)
N2 C27 C28 . . 109.14(18)
C30 C27 C28 . . 107.6(2)
C29 C27 C28 . . 109.50(19)
C27 C28 H28A . . 109.5
C27 C28 H28B . . 109.5
H28A C28 H28B . . 109.5
C27 C28 H28C . . 109.5
H28A C28 H28C . . 109.5
H28B C28 H28C . . 109.5
C27 C29 H29A . . 109.5
C27 C29 H29B . . 109.5
H29A C29 H29B . . 109.5
C27 C29 H29C . . 109.5
H29A C29 H29C . . 109.5
H29B C29 H29C . . 109.5
C27 C30 H30A . . 109.5
C27 C30 H30B . . 109.5
H30A C30 H30B . . 109.5
C27 C30 H30C . . 109.5
H30A C30 H30C . . 109.5
H30B C30 H30C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mn1 O1 . 2.1178(16)
Mn1 O4 2_756 2.1293(16)
Mn1 O6 . 2.2261(16)
Mn1 N3 . 2.2398(19)
Mn1 N1 . 2.268(2)
Mn1 N2 . 2.3927(19)
O1 C1 . 1.276(3)
O2 C1 . 1.252(3)
O3 C14 . 1.257(3)
O4 C14 . 1.269(3)
O4 Mn1 2_756 2.1294(16)
O5 C8 . 1.388(3)
O5 C5 . 1.397(3)
O6 H6A . 0.8782
O6 H6B . 0.8775
N1 C19 . 1.340(3)
N1 C15 . 1.348(3)
N2 C20 . 1.482(3)
N2 C21 . 1.490(3)
N2 C27 . 1.524(3)
N3 C22 . 1.341(3)
N3 C26 . 1.348(3)
C1 C2 . 1.504(3)
C2 C7 . 1.387(3)
C2 C3 . 1.392(3)
C3 C4 . 1.380(3)
C3 H3 . 0.95
C4 C5 . 1.383(3)
C4 H4 . 0.95
C5 C6 . 1.376(3)
C6 C7 . 1.394(3)
C6 H6 . 0.95
C7 H7 . 0.95
C8 C9 . 1.383(3)
C8 C13 . 1.391(3)
C9 C10 . 1.392(3)
C9 H9 . 0.95
C10 C11 . 1.392(3)
C10 H10 . 0.95
C11 C12 . 1.395(3)
C11 C14 . 1.506(3)
C12 C13 . 1.386(3)
C12 H12 . 0.95
C13 H13 . 0.95
C15 C16 . 1.378(3)
C15 H15 . 0.95
C16 C17 . 1.382(4)
C16 H16 . 0.95
C17 C18 . 1.389(4)
C17 H17 . 0.95
C18 C19 . 1.384(3)
C18 H18 . 0.95
C19 C20 . 1.515(3)
C20 H20A . 0.99
C20 H20B . 0.99
C21 C22 . 1.509(3)
C21 H21A . 0.99
C21 H21B . 0.99
C22 C23 . 1.392(3)
C23 C24 . 1.379(3)
C23 H23 . 0.95
C24 C25 . 1.386(3)
C24 H24 . 0.95
C25 C26 . 1.378(3)
C25 H25 . 0.95
C26 H26 . 0.95
C27 C30 . 1.528(3)
C27 C29 . 1.534(3)
C27 C28 . 1.535(3)
C28 H28A . 0.98
C28 H28B . 0.98
C28 H28C . 0.98
C29 H29A . 0.98
C29 H29B . 0.98
C29 H29C . 0.98
C30 H30A . 0.98
C30 H30B . 0.98
C30 H30C . 0.98
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O6 H6A O3 2_756 0.88 1.94 2.702(2) 143.9
O6 H6B O2 . 0.88 1.91 2.681(2) 145.8
