Ligand Control of Manganese Telluride Molecular Cluster Core Nuclearity.
Choi, Bonnie; Paley, Daniel W.; Siegrist, Theo; Steigerwald, Michael L.; Roy, Xavier; Inorganic chemistry 54 (2015) 8348–8355; doi:10.1021/acs.inorgchem.5b01020

data_4346232
_publ_section_title
;
 Ligand Control of Manganese Telluride Molecular Cluster Core Nuclearity.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8348
_journal_page_last               8355
_journal_paper_doi               10.1021/acs.inorgchem.5b01020
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C66 H120 Mn8 N12 Te8, 3(C7 H8)'
_chemical_formula_sum            'C87 H144 Mn8 N12 Te8'
_chemical_formula_weight         2818.45
_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     direct
_audit_creation_date             2014-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                61.056(5)
_cell_angle_beta                 83.162(4)
_cell_angle_gamma                87.953(3)
_cell_formula_units_Z            1
_cell_length_a                   14.1776(4)
_cell_length_b                   14.6358(7)
_cell_length_c                   14.9029(8)
_cell_measurement_reflns_used    9960
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.2980
_cell_measurement_theta_min      4.3470
_cell_volume                     2686.0(2)
_computing_cell_refinement
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_data_collection
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_data_reduction
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
  1 omega  -15.00   13.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000   30.0000 28

  2 omega   57.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910 -178.0000  -30.0000 44

  3 omega  -22.00    6.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000  -30.0000 28

  4 omega   16.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000  150.0000 36

  5 omega   67.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   57.0000  -60.0000 25

  6 omega   55.00   80.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910 -178.0000   30.0000 25

  7 omega   33.00   61.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   19.0000   30.0000 28

  8 omega   30.00   56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000  120.0000 26

  9 omega   62.00  100.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000  120.0000 38

 10 omega   64.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   37.0000 -120.0000 27

 11 omega   28.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   74.0000   55.4803 43

 12 omega  -28.00    0.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000 -120.0000 28

 13 omega   81.00  106.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   19.0000  -90.0000 25

 14 omega   12.00   41.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   19.0000  -90.0000 29

 15 omega  -16.00   27.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -44.0000 -153.0870 43

 16 omega   79.00  106.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   19.0000   90.0000 27

 17 omega   14.00   39.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   19.0000  -30.0000 25

 18 omega   22.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000  150.0000 27

 19 omega   56.00   84.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000  -30.0000 28

 20 omega   14.00   71.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -99.0000  -30.0000 57

 21 omega  -19.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -37.0000  -60.0000 49

 22 omega  -30.00   -1.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -37.0000 -180.0000 29

 23 omega    4.00   38.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -99.0000  -60.0000 34

 24 omega   62.00   93.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   57.0000  -90.0000 31

 25 omega   27.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000  -60.0000 25

 26 omega  -32.00   -4.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000  -60.0000 28

 27 omega   59.00   98.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   57.0000  120.0000 39

 28 omega  -10.00   18.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000    0.0000 28

 29 omega   27.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -57.0000    0.0000 25

 30 omega   23.00   74.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   37.0000   90.0000 51

 31 omega    8.00   33.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   11.0000   78.5198 25

 32 omega   31.00   56.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -32.0000 -169.1704 25

 33 omega    2.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -19.0000    0.0000 28

 34 omega  -22.00    6.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -19.0000  -30.0000 28

 35 omega  -24.00   16.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -19.0000 -150.0000 40

 36 omega   27.00   52.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -19.0000 -150.0000 25

 37 omega   11.00   36.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000  120.0000 25

 38 omega   78.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  178.0000 -180.0000 25

 39 omega   73.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   11.0000   78.5198 30

 40 omega  -29.00    6.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910    0.0000  -30.0000 35

 41 omega   66.00   95.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910    0.0000  -30.0000 29

 42 omega   39.00   67.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   57.0000   60.0000 28

 43 omega   44.00   74.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -99.0000 -120.0000 30

 44 omega   18.00   46.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   51.0000    7.1830 28

 45 omega   78.00  103.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   51.0000    7.1830 25

 46 omega   17.00   51.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   37.0000  -90.0000 34

 47 omega  -32.00    4.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -37.0000   90.0000 36

 48 omega   28.00   54.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -37.0000   90.0000 26

 49 omega   63.00   91.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000  -90.0000 28

 50 omega    8.00   36.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000   90.0000 28

 51 omega   52.00  102.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000   90.0000 50

 52 omega   10.00   44.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000  150.0000 34

 53 omega   61.00   89.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000  150.0000 28

 54 omega   20.00   59.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   57.0000  -30.0000 39

 55 omega   25.00  100.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   54.0000   19.7260 75

 56 omega   34.00   62.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   41.0000  -13.4816 28

 57 omega   74.00  104.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   41.0000  -13.4816 30

 58 omega   -6.00   22.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -37.0000  120.0000 28

 59 omega   25.00   50.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000 -180.0000 25

 60 omega   64.00   92.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910   77.0000   60.0000 28

 61 omega  -18.00   10.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000  -60.0000 28

 62 omega   19.00   45.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000  -60.0000 26

 63 omega   26.00   58.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000    0.0000 32

 64 omega    8.00   49.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910  -77.0000   30.0000 41

 65 omega   76.00  101.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       34.8910 -178.0000 -150.0000 25

 66 omega   78.00  109.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 31

 67 omega  137.00  178.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 41

 68 omega   70.00  164.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000   30.0000 94

 69 omega   76.00  121.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000   30.0000 45

 70 omega   39.00   94.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 55

 71 omega   46.00  100.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 54

 72 omega   86.00  133.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000 -150.0000 47

 73 omega  120.00  178.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 58

 74 omega   41.00   97.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 56

 75 omega   42.00  119.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -180.0000 77

 76 omega   70.00  170.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  120.0000 100

 77 omega  131.00  162.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -90.0000 31

 78 omega   38.00   63.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 25

 79 omega   61.00  115.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   90.0000 54

 80 omega   82.00  123.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -120.0000 41

 81 omega  103.00  175.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -60.0000 72

 82 omega   39.00   85.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 46

 83 omega   57.00   88.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 31

 84 omega   41.00   77.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 36

 85 omega   42.00   91.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 49

 86 omega   76.00  116.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 40

 87 omega   70.00   97.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000  -30.0000 27

 88 omega   43.00   71.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 28

 89 omega   52.00  108.00   1.0000   17.5000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -60.0000 56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0111988000
_diffrn_orient_matrix_UB_12      -0.0479101000
_diffrn_orient_matrix_UB_13      -0.0703050000
_diffrn_orient_matrix_UB_21      -0.0291622000
_diffrn_orient_matrix_UB_22      0.1068282000
_diffrn_orient_matrix_UB_23      -0.0844937000
_diffrn_orient_matrix_UB_31      0.1049231000
_diffrn_orient_matrix_UB_32      0.0277433000
_diffrn_orient_matrix_UB_33      -0.0454298000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            30272
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.505
_diffrn_reflns_theta_min         4.484
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    24.527
_exptl_absorpt_correction_T_max  0.677
_exptl_absorpt_correction_T_min  0.268
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'CrysAlisPro, Agilent Technologies, Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET) (compiled May 22 2014,16:03:01) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1366
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.998
_refine_diff_density_min         -1.092
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         10212
_refine_ls_number_restraints     696
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0515P)^2^+4.8868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7940
_reflns_number_total             10212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Mn8Te8_iPr2NHC6.cif
_cod_data_source_block           Mn8Te8-iPr2NHC-6
_cod_database_code               4346232
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C66 Mn8 N12 Te8 '
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 0.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(C103)=Sof(H103)=
 Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)=Sof(H106)=Sof(C107)=
 Sof(H107)=1-FVAR(1)
 Sof(C101)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C102)=Sof(C103)=Sof(H103)=
 Sof(C104)=Sof(H104)=Sof(C105)=Sof(H105)=Sof(C106)=Sof(H106)=Sof(C107)=
 Sof(H107)=FVAR(1)
 Fixed Sof: C101(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C102(0.5) C103(0.5)
 H103(0.5) C104(0.5) H104(0.5) C105(0.5) H105(0.5) C106(0.5) H106(0.5)
 C107(0.5) H107(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C21(H21), C33(H33), C41(H41), C53(H53), C61(H61)
5.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105), C106(H106), C107(H107), C103(H103),
 C104(H104), C105(H105), C106(H106), C107(H107), C103(H103), C104(H104),
 C105(H105), C106(H106), C107(H107)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C),
 C43(H43A,H43B,H43C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C),
 C101(H10A,H10B,H10C), C101(H10A,H10B,H10C), C101(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'