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_7712817
_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         'C72 H108 Mn18 N12 O58, 2(C2 H3 N), 2.5[C2H3N]'
_chemical_formula_sum            'C81 H121.5 Mn18 N16.5 O58'
_chemical_formula_weight         3243.36
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2022-06-17
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-29 deposited with the CCDC.	2023-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                103.925(2)
_cell_angle_beta                 99.153(2)
_cell_angle_gamma                117.635(2)
_cell_formula_units_Z            1
_cell_length_a                   15.1254(4)
_cell_length_b                   15.3885(4)
_cell_length_c                   15.9092(3)
_cell_measurement_reflns_used    26997
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9130
_cell_measurement_theta_min      4.4110
_cell_volume                     3022.25(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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   -112.00 -65.00   1.00    7.50    --  -41.79-144.00 179.00   47
  2  \w    -88.00  -7.00   1.00    7.50    --  -41.79 127.00  64.00   81
  3  \w   -101.00 -15.00   1.00    7.50    --  -41.79 144.00-126.00   86
  4  \w     29.00  98.00   1.00    7.50    --   41.79-127.00 -11.00   69
  5  \w     37.00 109.00   1.00    7.50    --   41.79-144.00 179.00   72
  6  \w     38.00 127.00   1.00   15.00    --  108.85-144.00 179.00   89
  7  \w     96.00 178.00   1.00   15.00    --  108.85 127.00  64.00   82
  8  \w     87.00 170.00   1.00   15.00    --  108.85 144.00-126.00   83
  9  \w     38.00 114.00   1.00   15.00    --  108.85-127.00 -11.00   76
 10  \w     -2.00  29.00   1.00    7.50    --   34.00  90.00 -45.66   31
 11  \w      2.00  29.00   1.00    7.50    --   38.00  90.00  55.21   27
 12  \w   -114.00 -19.00   1.00    7.50    --  -41.79 -38.00 -30.00   95
 13  \w   -114.00 -19.00   1.00    7.50    --  -41.79 -38.00  90.00   95
 14  \w     15.00 112.00   1.00    7.50    --   41.79  57.00-180.00   97
 15  \w     10.00  42.00   1.00    7.50    --   41.79  79.00 167.46   32
 16  \w     15.00  42.00   1.00    7.50    --   46.00  76.00 -80.88   27
 17  \w     13.00  42.00   1.00    7.50    --   46.00  82.00-139.70   29
 18  \w     13.00  42.00   1.00    7.50    --   46.00  82.00  67.84   29
 19  \w     14.00  42.00   1.00    7.50    --   46.00  80.00 -22.80   28
 20  \w     24.00 126.00   1.00    7.50    --   54.00  71.00-105.77  102
 21  \w     28.00 130.00   1.00    7.50    --   58.00  70.00 126.19  102
 22  \w     33.00 133.00   1.00    7.50    --   62.00  67.00  68.97  100
 23  \w     32.00 134.00   1.00    7.50    --   62.00  70.00-164.14  102
 24  \w     32.00 134.00   1.00    7.50    --   62.00  70.00  87.19  102
 25  \w     36.00 138.00   1.00    7.50    --   66.00  70.00-139.49  102
 26  \w     36.00 138.00   1.00    7.50    --   66.00  71.00  11.98  102
 27  \w     36.00 138.00   1.00    7.50    --   66.00  70.00 -44.49  102
 28  \w     37.00 137.00   1.00    7.50    --   66.00  69.00 161.55  100
 29  \w     40.00 142.00   1.00    7.50    --   70.00  71.00 -84.45  102
 30  \w     45.00 145.00   1.00    7.50    --   74.00  69.00 117.57  100
 31  \w     44.00 146.00   1.00    7.50    --   74.00  70.00 -21.80  102
 32  \w     50.00 148.00   1.00   15.00    --   78.00  61.00 108.85   98
 33  \w     48.00 150.00   1.00   15.00    --   78.00  71.00 164.47  102
 34  \w     50.00 148.00   1.00   15.00    --   78.00  61.00-149.85   98
 35  \w     50.00 149.00   1.00   15.00    --   78.00  65.00  55.73   99
 36  \w     48.00 150.00   1.00   15.00    --   78.00  71.00   7.32  102
 37  \w     54.00 152.00   1.00   15.00    --   82.00  61.00 -72.82   98
 38  \w     52.00 154.00   1.00   15.00    --   82.00  70.00 143.72  102
 39  \w     56.00 158.00   1.00   15.00    --   86.00  71.00-119.27  102
 40  \w     58.00 157.00   1.00   15.00    --   86.00  65.00-141.05   99
 41  \w     57.00 157.00   1.00   15.00    --   86.00  66.00  60.52  100
 42  \w     62.00 160.00   1.00   15.00    --   90.00  61.00 -51.15   98
 43  \w     67.00 164.00   1.00   15.00    --   94.00  58.00  95.48   97
 44  \w     67.00 164.00   1.00   15.00    --   94.00  57.00   6.91   97
 45  \w     69.00 169.00   1.00   15.00    --   98.00  69.00-177.32  100
 46  \w     74.00 173.00   1.00   15.00    --  102.00  65.00 109.18   99
 47  \w     75.00 172.00   1.00   15.00    --  102.00  57.00-133.81   97
 48  \w     72.00 174.00   1.00   15.00    --  102.00  70.00  12.29  102
 49  \w     37.00 113.00   1.00   15.00    --  108.85-125.00  30.00   76
 50  \w     81.00 178.00   1.00   15.00    --  108.85  61.00 -90.00   97
 51  \w     81.00 178.00   1.00   15.00    --  108.85  61.00  30.00   97
 52  \w     81.00 178.00   1.00   15.00    --  108.85  61.00  60.00   97
 53  \w     81.00 178.00   1.00   15.00    --  108.85  61.00 120.00   97
 54  \w     28.00 106.00   1.00   15.00    --  108.85 -94.00  30.00   78
 55  \w     81.00 178.00   1.00   15.00    --  108.85  61.00  90.00   97
 56  \w     37.00 113.00   1.00   15.00    --  108.85-125.00 120.00   76
 57  \w     81.00 178.00   1.00   15.00    --  108.85  61.00 -60.00   97
 58  \w     81.00 178.00   1.00   15.00    --  108.85  61.00 -30.00   97
 59  \w     39.00 136.00   1.00   15.00    --  108.85 -61.00 120.00   97
 60  \w     81.00 178.00   1.00   15.00    --  108.85  61.00-120.00   97
 61  \w     81.00 178.00   1.00   15.00    --  108.85  61.00 150.00   97
 62  \w     37.00 113.00   1.00   15.00    --  108.85-125.00 -60.00   76
 63  \w     28.00 106.00   1.00   15.00    --  108.85 -94.00-180.00   78
 64  \w      3.00  31.00   1.00    7.50    --   38.00  87.00-154.86   28
 65  \w   -114.00 -19.00   1.00    7.50    --  -41.79 -38.00-120.00   95
 66  \w     14.00  42.00   1.00    7.50    --   46.00  79.00 170.23   28
 67  \w     28.00 130.00   1.00    7.50    --   58.00  70.00 -63.33  102
 68  \w     28.00 130.00   1.00    7.50    --   58.00  71.00 163.50  102
 69  \w     28.00 104.00   1.00    7.50    --   58.00  71.00 -38.74   76
 70  \w     29.00 129.00   1.00    7.50    --   58.00  68.00   1.21  100
 71  \w     41.00 141.00   1.00    7.50    --   70.00  68.00 -96.84  100
 72  \w     41.00 141.00   1.00    7.50    --   70.00  69.00  58.83  100
 73  \w     46.00 144.00   1.00    7.50    --   74.00  64.00  89.86   98
 74  \w     45.00 145.00   1.00    7.50    --   74.00  67.00-172.41  100
 75  \w     45.00 145.00   1.00    7.50    --   74.00  66.00 -67.25  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Oxford Diffraction SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0787742000
_diffrn_orient_matrix_UB_12      -0.0372642000
_diffrn_orient_matrix_UB_13      -0.0940507000
_diffrn_orient_matrix_UB_21      0.0642980000
_diffrn_orient_matrix_UB_22      -0.0376050000
_diffrn_orient_matrix_UB_23      -0.0465188000
_diffrn_orient_matrix_UB_31      -0.0658178000
_diffrn_orient_matrix_UB_32      -0.1089132000
_diffrn_orient_matrix_UB_33      0.0062254000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1085
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            128161
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         3.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    15.573
_exptl_absorpt_correction_T_max  0.45696
_exptl_absorpt_correction_T_min  0.40744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Spherical absorption correction
using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       plate
_exptl_crystal_F_000             1637
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of diethyl ether and acetonitrile  by vapour diffusion'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_size_rad          0.040
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         11063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0691P)^2^+1.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7805
_reflns_number_total             11063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00732d2.cif
_cod_data_source_block           eb22077
_cod_original_cell_volume        3022.24(14)
_cod_original_formula_sum        'C81 H121.50 Mn18 N16.50 O58'
_cod_database_code               7712817
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C80 H132 Mn18 N16 O58'
_chemical_oxdiff_usercomment     '@ 120 K EA315_Et2O'
_shelx_estimated_absorpt_t_max   0.575
_shelx_estimated_absorpt_t_min   0.177
_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.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B), C18(H18A,H18B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C14(H14)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C22(H22A,H22B,
 H22C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 52 electrons were 
found in a volume of 350\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.5[C2H3N] per Formula Unit 
which account for 55 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72248
_shelx_hkl_checksum              46523
_shelx_fab_checksum              71297
_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 EA315_Et2O
_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 2.236
_oxdiff_exptl_absorpt_empirical_full_min 0.624