Seven-coordinate Mn(II) complex with a pyridine-based 15-membered macrocyclic ligand containing one acetate pendant arm: structure, stability and relaxation properties
Pražáková, Marie; Ndiaye, Daouda; Toth, Eva J.; Drahoš, Bohuslav; Dalton Transactions  (2023) –; doi:10.1039/D3DT00701D

data_7713008
_publ_section_title
;
 Seven-coordinate Mn(II) complex with a pyridine-based 15-membered
 macrocyclic ligand containing one acetate pendant arm: structure,
 stability and relaxation properties
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00701D
_journal_year                    2023
_chemical_formula_moiety         'Br Cl3 Mn, C30 H44 Mn2 N6 O8, 3(H2 O)'
_chemical_formula_sum            'C30 H50 Br Cl3 Mn3 N6 O11'
_chemical_formula_weight         1021.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-02-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-02-25 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7529(2)
_cell_length_b                   20.8862(4)
_cell_length_c                   18.2988(3)
_cell_measurement_reflns_used    9614
_cell_measurement_temperature    89.97(18)
_cell_measurement_theta_max      68.2150
_cell_measurement_theta_min      2.1153
_cell_volume                     4491.87(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.119a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     93.00 161.00   0.50    2.00    --   95.65  33.00  30.00  136
  2  \w    132.00 157.00   0.50    2.00    --   95.65  33.00-180.00   50
  3  \w     60.00 104.00   0.50    0.60    --   43.22  77.00-150.00   88
  4  \w     24.00  53.00   0.50    0.60    --   43.22  77.00-150.00   58
  5  \w    -72.00 -34.00   0.50    2.00    --  -94.09  68.00  30.00   76
  6  \w    -53.00 -28.00   0.50    2.00    --  -94.09  50.00 -60.00   50
  7  \w    -57.00 -31.00   0.50    2.00    --  -94.09  50.00 -90.00   52
  8  \w    -54.00 -28.00   0.50    2.00    --  -94.09  50.00-120.00   52
  9  \w    -94.00 -69.00   0.50    0.60    --  -41.66 157.00-158.00   50
 10  \w    -98.00 -73.00   0.50    0.60    --  -41.66 138.00-120.00   50
 11  \w    -63.00 -23.00   0.50    0.60    --  -41.66 138.00-120.00   80
 12  \w    -81.00 -32.00   0.50    0.60    --  -41.66 118.00  47.00   98
 13  \w    -17.00  19.00   0.50    0.60    --   43.22 -21.00 -60.00   72
 14  \w     30.00  79.00   0.50    2.00    --   95.65 -68.00 -90.00   98
 15  \w     39.00  64.00   0.50    2.00    --   95.65 -59.00 -60.00   50
 16  \w    -21.00  37.00   0.50    0.60    --   43.22 -32.00  60.00  116
 17  \w     52.00  85.00   0.50    0.60    --   43.22 157.00-158.00   66
 18  \w     64.00  90.00   0.50    0.60    --   43.22 138.00 -30.00   52
 19  \w     30.00  55.00   0.50    2.00    --   95.65 -50.00 -30.00   50
 20  \w     64.00 104.00   0.50    2.00    --   95.65-118.00 -38.00   80
 21  \w     57.00  83.00   0.50    0.60    --   43.22-157.00 166.00   52
 22  \w     57.00  82.00   0.50    2.00    --   95.65-157.00 166.00   50
 23  \w    -64.00 -31.00   0.50    2.00    --  -94.09 117.00-150.00   66
 24  \w   -108.00 -80.00   0.50    2.00    --  -94.09 117.00-150.00   56
 25  \w   -164.00 -77.00   0.50    2.00    --  -94.09 -17.00  30.00  174
 26  \w   -134.00 -88.00   0.50    2.00    --  -94.09-118.00 -38.00   92
 27  \w   -104.00 -70.00   0.50    0.60    --  -41.66 -43.00 120.00   68
 28  \w    -63.00 -31.00   0.50    0.60    --  -41.66 -43.00 120.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15874
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.345
_diffrn_reflns_theta_min         3.211
_exptl_absorpt_coefficient_mu    9.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       block
_exptl_crystal_F_000             2084
_exptl_crystal_size_max          0.243
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.124
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      15.580
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0532
_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/[\s^2^(Fo^2^)+(0.1071P)^2^+6.0213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3923
_reflns_number_total             4181
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00701d2.cif
_cod_data_source_block           01
_cod_database_code               7713008
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.373
_shelx_estimated_absorpt_t_min   0.197
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Cl2A-Mn2
 2.38 with sigma of 0.02
 Cl2-Mn2
 2.38 with sigma of 0.02
 Br1-Mn2 \\sim Br1A-Mn2
 with sigma of 0.02
 Cl2-Mn2 \\sim Cl2A-Mn2 \\sim Cl1_$1-Mn2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br1A) = Uanis(Br1)
Uanis(Cl2) = Uanis(Cl2A)
4. Others
 Sof(Br1A)=Sof(Cl2A)=0.5*(1-FVAR(2))
 Sof(Br1)=Sof(Cl2)=0.5*FVAR(2)
 Fixed Sof: H6C(0.5) H6D(0.5)
5.a Free rotating group:
 O5(H5A,H5B), O6(H6C,H6D)
5.b Ternary CH refined with riding coordinates:
 N3(H3)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C12(H12A,H12B), C10(H10A,H10B), C14(H14A,
 H14B), C6(H6A,H6B), C9(H9A,H9B), C7(H7A,H7B), C8(H8A,H8B)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C3(H3A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              7331
_shelx_fab_checksum              95872
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;