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_4346229
_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_absolute_configuration ad
_chemical_formula_moiety         'C28 H48 Mn4 N8 Te4, C H2 Cl2'
_chemical_formula_sum            'C29 H50 Cl2 Mn4 N8 Te4'
_chemical_formula_weight         1311.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5916(4)
_cell_length_b                   19.4968(15)
_cell_length_c                   23.8118(14)
_cell_measurement_reflns_used    6632
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.2450
_cell_measurement_theta_min      4.3700
_cell_volume                     4452.9(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega   57.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000 -180.0000 51

  2 omega   55.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316 -178.0000  -60.0000 53

  3 omega   57.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000    0.0000 51

  4 omega   57.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000   90.0000 51

  5 omega   57.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000   60.0000 51

  6 omega   55.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316 -178.0000   30.0000 53

  7 omega   55.00  108.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316 -178.0000  -30.0000 53

  8 omega    1.00   74.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -99.0000 -180.0000 73

  9 omega   38.00   91.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 53

 10 omega   81.00  176.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 95

 11 omega   40.00  135.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  -30.0000 95

 12 omega   37.00   99.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -22.0000  -90.1809 62

 13 omega   38.00   91.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -90.0000 53

 14 omega  100.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   60.0000 78

 15 omega   38.00   91.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 16 omega   39.00  109.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -30.0000 70

 17 omega   70.00  178.00   1.0000   18.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000 -180.0000 108
;
_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      0.0068326000
_diffrn_orient_matrix_UB_12      -0.0740201000
_diffrn_orient_matrix_UB_13      -0.0224108000
_diffrn_orient_matrix_UB_21      -0.1508612000
_diffrn_orient_matrix_UB_22      0.0063922000
_diffrn_orient_matrix_UB_23      -0.0216186000
_diffrn_orient_matrix_UB_31      0.0547886000
_diffrn_orient_matrix_UB_32      0.0266965000
_diffrn_orient_matrix_UB_33      -0.0567453000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23035
_diffrn_reflns_point_group_measured_fraction_full 0.949
_diffrn_reflns_point_group_measured_fraction_max 0.904
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.570
_diffrn_reflns_theta_min         4.351
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.623
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.159
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.957
_exptl_crystal_description
;
;
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.1175
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.0218
_refine_diff_density_max         2.272
_refine_diff_density_min         -2.257
_refine_diff_density_rms         0.252
_refine_ls_abs_structure_details
;
 Flack x determined using 2028 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         8095
_refine_ls_number_restraints     568
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0854
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1364P)^2^+30.1181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2236
_refine_ls_wR_factor_ref         0.2403
_reflns_Friedel_coverage         0.683
_reflns_Friedel_fraction_full    0.886
_reflns_Friedel_fraction_max     0.829
_reflns_number_gt                6691
_reflns_number_total             8095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Mn4Te4_Me2NHC4.cif
_cod_data_source_block           Mn4Te4-Me2NHC-4
_cod_database_code               4346229
_chemical_oxdiff_formula         'c27 h48 Mn4 N8 Te4 '
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C81-Cl82 = C81-Cl83
 1.76 with sigma of 0.02
 Cl82-Cl83
 2.93 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C3, C5, C6, C7, C8, C9, C11, C23, C25, C26, C27, C28, C29, C31, C43, C45, C46,
  C47, C48, C49, C51, C63, C65, C66, C67, C68, C69, C71, C81, N4, N10, N24, N30,
  N44, N50, N64, N70, Cl82, Cl83
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{C3, N10, C11, C8, C9, C6, C7, N4, C5} sigma for 1-2: 0.02, 1-3: 0.04
{C23, N24, C25, C26, C27, C28, C29, N30, C31} sigma for 1-2: 0.02, 1-3: 0.04
{C43, N44, C45, C46, C47, C48, C49, N50, C51} sigma for 1-2: 0.02, 1-3: 0.04
{C63, N64, C65, C66, C67, C68, C69, N70, C71} sigma for 1-2: 0.02, 1-3: 0.04
{C23, N30, C31, C28, C29, C26, C27, N24, C25} sigma for 1-2: 0.02, 1-3: 0.04
{C43, N50, C51, C48, C49, C46, C47, N44, C45} sigma for 1-2: 0.02, 1-3: 0.04
{C63, N70, C71, C68, C69, C66, C67, N64, C65} sigma for 1-2: 0.02, 1-3: 0.04
as
{C3, N4, C5, C6, C7, C8, C9, N10, C11}
5.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B)
5.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C),
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C69(H69A,H69B,H69C),
 C71(H71A,H71B,H71C)
;
_shelx_res_checksum              7720
_shelx_hkl_checksum              2183
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'