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_4346235
_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         'C36 H90 Mn6 P6 Te6'
_chemical_formula_sum            'C36 H90 Mn6 P6 Te6'
_chemical_formula_weight         1804.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-10-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.8798(6)
_cell_length_b                   14.5239(4)
_cell_length_c                   22.4484(7)
_cell_measurement_reflns_used    9318
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.4510
_cell_measurement_theta_min      5.7670
_cell_volume                     6807.6(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   57.00  108.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000  120.0000 51

  2 omega   19.00  103.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316   57.0000 -180.0000 84

  3 omega   57.00  108.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000    0.0000 51

  4 omega  -32.00   52.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -57.0000  150.0000 84

  5 omega   57.00  108.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000  -30.0000 51

  6 omega   57.00  108.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316  178.0000 -120.0000 51

  7 omega    1.00   74.00   1.0000    3.2700
omega____ theta____ kappa____ phi______ frames
    -       35.5316  -99.0000  150.0000 73

  8 omega   87.00  178.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000  -30.0000 91

  9 omega   39.00  109.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 10 omega   38.00   91.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  150.0000 53

 11 omega   90.00  175.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -90.0000 85

 12 omega   90.00  175.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000   60.0000 85

 13 omega   39.00  109.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 70

 14 omega   91.00  176.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  120.0000 85

 15 omega  100.00  171.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 71

 16 omega   54.00   81.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 27

 17 omega   39.00   66.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   30.0000 27

 18 omega   39.00   78.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 39

 19 omega   58.00   84.00   1.0000   13.0800
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 26
;
_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      0.0156661000
_diffrn_orient_matrix_UB_12      0.0303973000
_diffrn_orient_matrix_UB_13      -0.0641149000
_diffrn_orient_matrix_UB_21      -0.0606089000
_diffrn_orient_matrix_UB_22      -0.0493648000
_diffrn_orient_matrix_UB_23      -0.0226331000
_diffrn_orient_matrix_UB_31      -0.0391601000
_diffrn_orient_matrix_UB_32      0.0887210000
_diffrn_orient_matrix_UB_33      0.0093165000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18021
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.642
_diffrn_reflns_theta_min         5.413
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    30.153
_exptl_absorpt_correction_T_max  0.471
_exptl_absorpt_correction_T_min  0.075
_exptl_absorpt_correction_type   gaussian
_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) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description
;
;
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.1637
_exptl_crystal_size_mid          0.0918
_exptl_crystal_size_min          0.0479
_refine_diff_density_max         1.084
_refine_diff_density_min         -0.703
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.493(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         6276
_refine_ls_number_restraints     193
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0388P)^2^+14.9037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                6039
_reflns_number_total             6276
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Mn6Te6_PEt36.cif
_cod_data_source_block           Mn6Te6-PEt3-6
_cod_original_cell_volume        6807.6(4)
_cod_database_code               4346235
_chemical_oxdiff_formula         Mn6Te6P6C36
_platon_squeeze_void_probe_radius 1.20
_reflns_odcompleteness_completeness 99.82
_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. Uiso/Uaniso restraints and constraints
P52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
P72 \\sim C73 \\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C54) = Uanis(C58)
3. Rigid body (RIGU) restrains
 P52, C53, C54, C55, C56, C57, C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P72, C73, C74, C75, C76, C77, C78
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Same fragment restrains
{Mn71, P72, C73, C74, C75, C76, C77, C78}
{Mn51, P52, C53, C54, C55, C56, C57, C58}
as
{Mn11, P12, C13, C14, C15, C16, C17, C18}
5. Others
 Fixed Sof: C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5)
 H54C(0.5) C55(0.5) H55A(0.5) H55B(0.5) C56(0.5) H56A(0.5) H56B(0.5) H56C(0.5)
 C57(0.5) H57A(0.5) H57B(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C73(0.5)
 H73A(0.5) H73B(0.5) C74(0.5) H74A(0.5) H74B(0.5) H74C(0.5) C75(0.5) H75A(0.5)
 H75B(0.5) C76(0.5) H76A(0.5) H76B(0.5) H76C(0.5) C77(0.5) H77A(0.5) H77B(0.5)
 C78(0.5) H78A(0.5) H78B(0.5) H78C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C33(H33A,H33B), C35(H35A,
 H35B), C37(H37A,H37B), C53(H53A,H53B), C55(H55A,H55B), C57(H57A,H57B),
 C73(H73A,H73B), C75(H75A,H75B), C77(H77A,H77B)
6.b Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C74(H74A,H74B,
 H74C), C76(H76A,H76B,H76C), C78(H78A,H78B,H78C)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              37782
_shelx_hkl_checksum              63815
_shelx_fab_checksum              29806
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'