#------------------------------------------------------------------------------
#$Date: 2024-02-04 13:36:17 +0200 (Sun, 04 Feb 2024) $
#$Revision: 289435 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247747.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_7247747
loop_
_publ_author_name
'Kumar, Jayasree'
'Tarannum, Ibtesham'
'Zheng, Yan-Zhen'
'Singh, Saurabh Kumar'
'Mondal, Kartik Chandra'
_publ_section_title
;
 Assembly of MnIII ions into di-, tetra-, deca-nuclear coordination
 complexes, zero- to three-dimensional molecular frameworks: molecular
 spin flop to and short-range bulk magnetic spin flop ordering
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              80
_journal_page_last               99
_journal_paper_doi               10.1039/D3CE00967J
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C30 H32 Mn2 N6 O8'
_chemical_formula_sum            'C30 H32 Mn2 N6 O8'
_chemical_formula_weight         714.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2023-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                94.868(2)
_cell_angle_beta                 105.897(2)
_cell_angle_gamma                94.543(2)
_cell_formula_units_Z            1
_cell_length_a                   7.8214(5)
_cell_length_b                   9.9952(6)
_cell_length_c                   10.4841(7)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      3.04
_cell_volume                     780.92(9)
_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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            23839
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.902
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       Block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2742
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0478
_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)+(0.0606P)²+1.5027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2235
_reflns_number_total             2742
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3ce00967j2.cif
_cod_data_source_block           JS10
_cod_depositor_comments
'Adding full bibliography for 7247746--7247749.cif.'
_cod_database_code               7247747
_shelx_shelxl_version_number     2018/3
_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   0.881
_shelx_estimated_absorpt_t_max   0.918
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.56326(8) 0.52502(5) 0.37249(6) 0.0330(2) Uani 1 1 d . . . . .
O1 O 0.4636(4) 0.6873(3) 0.3341(3) 0.0386(6) Uani 1 1 d . . . . .
O2 O 0.6680(4) 0.3567(2) 0.3767(3) 0.0366(6) Uani 1 1 d . . . . .
O3 O 0.6575(3) 0.5732(2) 0.5594(2) 0.0318(6) Uani 1 1 d . . . . .
O4 O 0.7952(4) 0.6160(3) 0.3098(3) 0.0426(7) Uani 1 1 d . . . . .
H4A H 0.792242 0.698156 0.299000 0.064 Uiso 1 1 calc R U . . .
N1 N 0.4527(4) 0.4434(3) 0.1854(3) 0.0325(7) Uani 1 1 d . . . . .
N2 N 0.4991(5) 0.3135(3) 0.1540(3) 0.0378(8) Uani 1 1 d . . . . .
N3 N 0.7704(5) -0.1180(3) 0.2681(4) 0.0501(10) Uani 1 1 d . . . . .
C1 C 0.3390(5) 0.4930(4) 0.0924(4) 0.0362(9) Uani 1 1 d . . . . .
H1 H 0.295012 0.440780 0.007798 0.043 Uiso 1 1 calc R U . . .
C2 C 0.2743(5) 0.6232(4) 0.1089(4) 0.0375(9) Uani 1 1 d . . . . .
C3 C 0.1376(6) 0.6601(5) 0.0032(5) 0.0488(11) Uani 1 1 d . . . . .
H2 H 0.092880 0.599213 -0.075945 0.059 Uiso 1 1 calc R U . . .
C4 C 0.0672(7) 0.7808(5) 0.0107(5) 0.0578(13) Uani 1 1 d . . . . .
H3 H -0.028255 0.802114 -0.060162 0.069 Uiso 1 1 calc R U . . .
C5 C 0.1394(7) 0.8717(5) 0.1253(5) 0.0533(12) Uani 1 1 d . . . . .
H4 H 0.094526 0.956884 0.130973 0.064 Uiso 1 1 calc R U . . .
C6 C 0.2734(6) 0.8407(4) 0.2294(5) 0.0422(10) Uani 1 1 d . . . . .
H5 H 0.321479 0.905540 0.305130 0.051 Uiso 1 1 calc R U . . .
C7 C 0.3419(5) 0.7136(4) 0.2266(4) 0.0388(9) Uani 1 1 d . . . . .
C8 C 0.6085(5) 0.2803(4) 0.2618(4) 0.0354(9) Uani 1 1 d . . . . .
C9 C 0.6693(5) 0.1431(4) 0.2612(4) 0.0366(9) Uani 1 1 d . . . . .
C10 C 0.7357(6) 0.0921(4) 0.3819(5) 0.0468(11) Uani 1 1 d . . . . .
H9 H 0.748076 0.145103 0.464095 0.056 Uiso 1 1 calc R U . . .
C11 C 0.7834(7) -0.0382(4) 0.3792(5) 0.0535(12) Uani 1 1 d . . . . .
H8 H 0.828294 -0.072940 0.462042 0.064 Uiso 1 1 calc R U . . .
C12 C 0.7094(6) -0.0664(4) 0.1535(5) 0.0509(12) Uani 1 1 d . . . . .
H7 H 0.700719 -0.121221 0.072890 0.061 Uiso 1 1 calc R U . . .
C13 C 0.6578(6) 0.0625(4) 0.1449(4) 0.0432(10) Uani 1 1 d . . . . .
H6 H 0.615195 0.094956 0.060535 0.052 Uiso 1 1 calc R U . . .
C14 C 0.7451(6) 0.7028(4) 0.6129(4) 0.0413(10) Uani 1 1 d . . . . .
H12 H 0.662677 0.770847 0.585902 0.062 Uiso 1 1 calc R U . . .
H10 H 0.849285 0.719863 0.579392 0.062 Uiso 1 1 calc R U . . .
H11 H 0.784367 0.707869 0.710463 0.062 Uiso 1 1 calc R U . . .
C15 C 0.9732(6) 0.5846(4) 0.3385(5) 0.0474(11) Uani 1 1 d . . . . .
H13 H 0.976200 0.488084 0.347996 0.071 Uiso 1 1 calc R U . . .
H14 H 1.044370 0.637306 0.421926 0.071 Uiso 1 1 calc R U . . .
H15 H 1.022786 0.606706 0.265669 0.071 Uiso 1 1 calc R 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
_geom_angle_publ_flag
O1 Mn1 O3 96.46(11) . . ?
O1 Mn1 O2 168.87(12) . . ?
O3 Mn1 O2 93.51(11) . . ?
O1 Mn1 N1 91.07(12) . . ?
O3 Mn1 N1 170.07(12) . . ?
O2 Mn1 N1 79.63(12) . . ?
O1 Mn1 O3 97.41(11) . 2_666 ?
O3 Mn1 O3 80.59(10) . 2_666 ?
O2 Mn1 O3 89.10(11) . 2_666 ?
N1 Mn1 O3 92.05(11) . 2_666 ?
O1 Mn1 O4 85.54(11) . . ?
O3 Mn1 O4 98.08(11) . . ?
O2 Mn1 O4 88.16(11) . . ?
N1 Mn1 O4 88.93(12) . . ?
O3 Mn1 O4 176.87(9) 2_666 . ?
O1 Mn1 Mn1 99.13(9) . 2_666 ?
O3 Mn1 Mn1 44.19(8) . 2_666 ?
O2 Mn1 Mn1 91.47(9) . 2_666 ?
N1 Mn1 Mn1 128.15(10) . 2_666 ?
O3 Mn1 Mn1 36.39(6) 2_666 2_666 ?
O4 Mn1 Mn1 142.20(8) . 2_666 ?
C7 O1 Mn1 129.4(2) . . ?
C8 O2 Mn1 111.9(2) . . ?
C14 O3 Mn1 121.7(2) . . ?
C14 O3 Mn1 123.2(2) . 2_666 ?
Mn1 O3 Mn1 99.41(10) . 2_666 ?
C15 O4 Mn1 130.4(3) . . ?
C15 O4 H4A 109.5 . . ?
Mn1 O4 H4A 114.1 . . ?
C1 N1 N2 117.0(3) . . ?
C1 N1 Mn1 127.5(3) . . ?
N2 N1 Mn1 115.4(2) . . ?
C8 N2 N1 107.3(3) . . ?
C11 N3 C12 116.7(4) . . ?
N1 C1 C2 124.0(4) . . ?
N1 C1 H1 118.0 . . ?
C2 C1 H1 118.0 . . ?
C3 C2 C7 119.1(4) . . ?
C3 C2 C1 118.3(4) . . ?
C7 C2 C1 122.6(4) . . ?
C4 C3 C2 122.2(4) . . ?
C4 C3 H2 118.9 . . ?
C2 C3 H2 118.9 . . ?
C3 C4 C5 118.2(4) . . ?
C3 C4 H3 120.9 . . ?
C5 C4 H3 120.9 . . ?
C6 C5 C4 121.4(4) . . ?
C6 C5 H4 119.3 . . ?
C4 C5 H4 119.3 . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 H5 119.4 . . ?
C7 C6 H5 119.4 . . ?
O1 C7 C2 124.4(3) . . ?
O1 C7 C6 118.0(4) . . ?
C2 C7 C6 117.6(4) . . ?
N2 C8 O2 125.7(3) . . ?
N2 C8 C9 119.2(3) . . ?
O2 C8 C9 115.0(3) . . ?
C13 C9 C10 118.4(4) . . ?
C13 C9 C8 122.6(4) . . ?
C10 C9 C8 118.9(4) . . ?
C11 C10 C9 118.1(4) . . ?
C11 C10 H9 120.9 . . ?
C9 C10 H9 120.9 . . ?
N3 C11 C10 124.2(4) . . ?
N3 C11 H8 117.9 . . ?
C10 C11 H8 117.9 . . ?
N3 C12 C13 123.7(4) . . ?
N3 C12 H7 118.1 . . ?
C13 C12 H7 118.1 . . ?
C9 C13 C12 118.7(4) . . ?
C9 C13 H6 120.6 . . ?
C12 C13 H6 120.6 . . ?
O3 C14 H12 109.5 . . ?
O3 C14 H10 109.5 . . ?
H12 C14 H10 109.5 . . ?
O3 C14 H11 109.5 . . ?
H12 C14 H11 109.5 . . ?
H10 C14 H11 109.5 . . ?
O4 C15 H13 109.5 . . ?
O4 C15 H14 109.5 . . ?
H13 C15 H14 109.5 . . ?
O4 C15 H15 109.5 . . ?
H13 C15 H15 109.5 . . ?
H14 C15 H15 109.5 . . ?
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
Mn1 O1 1.881(3) . ?
Mn1 O3 1.900(3) . ?
Mn1 O2 1.927(2) . ?
Mn1 N1 1.987(3) . ?
Mn1 O3 2.232(3) 2_666 ?
Mn1 O4 2.246(3) . ?
Mn1 Mn1 3.1584(12) 2_666 ?
O1 C7 1.322(5) . ?
O2 C8 1.316(5) . ?
O3 C14 1.410(4) . ?
O4 C15 1.407(5) . ?
O4 H4A 0.8400 . ?
N1 C1 1.290(5) . ?
N1 N2 1.412(4) . ?
N2 C8 1.302(5) . ?
N3 C11 1.329(6) . ?
N3 C12 1.329(6) . ?
C1 C2 1.447(5) . ?
C1 H1 0.9500 . ?
C2 C3 1.411(6) . ?
C2 C7 1.413(6) . ?
C3 C4 1.371(6) . ?
C3 H2 0.9500 . ?
C4 C5 1.396(7) . ?
C4 H3 0.9500 . ?
C5 C6 1.366(6) . ?
C5 H4 0.9500 . ?
C6 C7 1.419(5) . ?
C6 H5 0.9500 . ?
C8 C9 1.487(5) . ?
C9 C13 1.380(6) . ?
C9 C10 1.386(6) . ?
C10 C11 1.382(6) . ?
C10 H9 0.9500 . ?
C11 H8 0.9500 . ?
C12 C13 1.383(6) . ?
C12 H7 0.9500 . ?
C13 H6 0.9500 . ?
C14 H12 0.9800 . ?
C14 H10 0.9800 . ?
C14 H11 0.9800 . ?
C15 H13 0.9800 . ?
C15 H14 0.9800 . ?
C15 H15 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Mn1 O1 C7 -163.0(3) . . . . ?
O2 Mn1 O1 C7 43.6(8) . . . . ?
N1 Mn1 O1 C7 10.5(3) . . . . ?
O3 Mn1 O1 C7 -81.7(3) 2_666 . . . ?
O4 Mn1 O1 C7 99.4(3) . . . . ?
Mn1 Mn1 O1 C7 -118.4(3) 2_666 . . . ?
O1 Mn1 O3 C14 -42.6(3) . . . . ?
O2 Mn1 O3 C14 132.5(3) . . . . ?
O3 Mn1 O3 C14 -139.0(3) 2_666 . . . ?
O4 Mn1 O3 C14 43.8(3) . . . . ?
Mn1 Mn1 O3 C14 -139.0(3) 2_666 . . . ?
O1 Mn1 O3 Mn1 96.47(12) . . . 2_666 ?
O2 Mn1 O3 Mn1 -88.50(11) . . . 2_666 ?
O3 Mn1 O3 Mn1 0.0 2_666 . . 2_666 ?
O4 Mn1 O3 Mn1 -177.13(9) . . . 2_666 ?
C1 N1 N2 C8 -177.5(3) . . . . ?
Mn1 N1 N2 C8 -0.3(4) . . . . ?
N2 N1 C1 C2 178.6(3) . . . . ?
Mn1 N1 C1 C2 1.8(6) . . . . ?
N1 C1 C2 C3 -174.2(4) . . . . ?
N1 C1 C2 C7 5.4(6) . . . . ?
C7 C2 C3 C4 -0.2(7) . . . . ?
C1 C2 C3 C4 179.3(4) . . . . ?
C2 C3 C4 C5 2.7(7) . . . . ?
C3 C4 C5 C6 -1.8(7) . . . . ?
C4 C5 C6 C7 -1.4(7) . . . . ?
Mn1 O1 C7 C2 -7.1(6) . . . . ?
Mn1 O1 C7 C6 172.4(3) . . . . ?
C3 C2 C7 O1 176.7(4) . . . . ?
C1 C2 C7 O1 -2.9(6) . . . . ?
C3 C2 C7 C6 -2.9(6) . . . . ?
C1 C2 C7 C6 177.5(4) . . . . ?
C5 C6 C7 O1 -175.8(4) . . . . ?
C5 C6 C7 C2 3.7(6) . . . . ?
N1 N2 C8 O2 -2.0(5) . . . . ?
N1 N2 C8 C9 175.4(3) . . . . ?
Mn1 O2 C8 N2 3.3(5) . . . . ?
Mn1 O2 C8 C9 -174.2(3) . . . . ?
N2 C8 C9 C13 18.7(6) . . . . ?
O2 C8 C9 C13 -163.7(4) . . . . ?
N2 C8 C9 C10 -159.4(4) . . . . ?
O2 C8 C9 C10 18.2(5) . . . . ?
C13 C9 C10 C11 -1.3(6) . . . . ?
C8 C9 C10 C11 176.8(4) . . . . ?
C12 N3 C11 C10 0.9(7) . . . . ?
C9 C10 C11 N3 0.3(7) . . . . ?
C11 N3 C12 C13 -0.9(7) . . . . ?
C10 C9 C13 C12 1.3(6) . . . . ?
C8 C9 C13 C12 -176.8(4) . . . . ?
N3 C12 C13 C9 -0.1(7) . . . . ?
