Tetra-, tetradeca- and octadecametallic clusters of Mn
Brechin, Euan K.; Agapaki, Eleftheria; Canaj, Angelos; Nichol, Gary Stephen; Dalton Transactions  (2023) –; doi:10.1039/D3DT00732D

data_7712815
_publ_section_title
;
 Tetra-, tetradeca- and octadecametallic clusters of Mn
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00732D
_journal_year                    2023
_chemical_formula_moiety
'C24 H44 Br4 Mn4 N8 O8, 2(C2 H3 N), [+ solvents]'
_chemical_formula_sum            'C28.5 H50.75 Br4 Mn4 N10.25 O8'
_chemical_formula_weight         1204.44
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-14
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-12-29 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                99.820(2)
_cell_angle_beta                 90.437(2)
_cell_angle_gamma                105.874(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1989(2)
_cell_length_b                   12.8405(3)
_cell_length_c                   18.4168(3)
_cell_measurement_reflns_used    29932
_cell_measurement_temperature    120.00(11)
_cell_measurement_theta_max      32.4360
_cell_measurement_theta_min      3.7190
_cell_volume                     2282.13(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.929
_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    -83.00  -6.00   1.00   10.00    --  -24.07 134.00 -49.00   77
  2  \w    -83.00  -6.00   1.00   10.00    --  -24.07 135.00 129.00   77
  3  \w      6.00  85.00   1.00   10.00    --   25.94-135.00  63.00   79
  4  \w      6.00  85.00   1.00   10.00    --   25.94-134.00-116.00   79
  5  \w    -91.00  -7.00   1.00   10.00    --  -24.07 -57.00  30.00   84
  6  \w    -95.00   5.00   1.00   10.00    --  -24.07 -19.00  30.00  100
  7  \w    -93.00  -5.00   1.00   10.00    --  -24.07 -38.00  60.00   88
  8  \w    -20.00  65.00   1.00   10.00    --   25.94 -99.00 120.00   85
  9  \w      7.00  95.00   1.00   10.00    --   25.94  38.00-150.00   88
 10  \w    -20.00  65.00   1.00   10.00    --   25.94 -99.00 -60.00   85
 11  \w     -3.00  97.00   1.00   10.00    --   25.94  19.00  30.00  100
 12  \w      9.00  93.00   1.00   10.00    --   25.94  57.00 -60.00   84
 13  \w     35.00  99.00   1.00   10.00    --   25.94-178.00 -30.00   64
 14  \w    -43.00  39.00   1.00   10.00    --  -24.07  38.00 120.00   82
 15  \w      9.00  93.00   1.00   10.00    --   25.94  57.00 150.00   84
 16  \w      9.00  93.00   1.00   10.00    --   25.94  57.00  30.00   84
 17  \w      9.00  93.00   1.00   10.00    --   25.94  57.00-120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0050093000
_diffrn_orient_matrix_UB_12      -0.0546099000
_diffrn_orient_matrix_UB_13      0.0047162000
_diffrn_orient_matrix_UB_21      -0.0052008000
_diffrn_orient_matrix_UB_22      -0.0172472000
_diffrn_orient_matrix_UB_23      -0.0388650000
_diffrn_orient_matrix_UB_31      0.0720620000
_diffrn_orient_matrix_UB_32      0.0113234000
_diffrn_orient_matrix_UB_33      -0.0002234000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            87672
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.847
_diffrn_reflns_theta_min         3.327
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.636
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38030
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             1195
_exptl_crystal_recrystallization_method
'The material was recrystallised from acetonitrile by slow evaporation'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         15804
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+1.4328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12560
_reflns_number_total             15804
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00732d2.cif
_cod_data_source_block           eb21266
_cod_original_formula_sum        'C28.50 H50.75 Br4 Mn4 N10.25 O8'
_cod_database_code               7712815
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 O10 N10 Mn4 Br4'
_chemical_oxdiff_usercomment     '@ 120 K EA205'
_shelx_estimated_absorpt_t_max   0.737
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{N11, C30}
3. Uiso/Uaniso restraints and constraints
Uanis(N11) = Uanis(C30)
4. Rigid body (RIGU) restrains
 N11, C29, C30
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N11(0.25) C30(0.25) H11D(0.25) H11E(0.25) H11F(0.25) C29(0.25)
6.a Everything fixed:
 H11D, H11E, H11F
6.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C10(H10A,H10B), C16(H16A,H16B), C22(H22A,H22B)
6.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C14(H14), C20(H20)
6.d Idealised Me refined as rotating group:
 C5(H5C,H5D,H5E), C6(H6C,H6D,H6E), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              23437
_shelx_hkl_checksum              48834
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems Cryostream 700+'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id EA205
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.228
_oxdiff_exptl_absorpt_empirical_full_min 0.717