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_4346230
_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         'c18 h54 mn6 p6 te6, C H2 Cl2'
_chemical_formula_sum            'C19 H56 Cl2 Mn6 P6 Te6'
_chemical_formula_weight         1636.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-12
_audit_creation_method
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Olex2 1.2
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_cell_formula_units_Z            16
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_cell_measurement_reflns_used    19251
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_cell_volume                     21287.1(8)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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_diffrn_measured_fraction_theta_full 0.998
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_diffrn_measurement_details
;
  1 omega   35.00   89.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  178.0000   90.0000 108

  2 phi    254.00  289.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
  17.1930   17.1930  -40.0000     -     70

  3 omega  -54.00   47.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -19.0000  150.0000 202

  4 omega  -10.00   85.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   77.0000 -180.0000 190

  5 omega   34.00   90.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930 -178.0000 -180.0000 112

  6 omega  -52.00   36.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930  -37.0000 -120.0000 176

  7 omega    0.00   37.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   57.0000   60.0000 74

  8 omega   -2.00   86.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1930   37.0000  -30.0000 176
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_diffrn_reflns_number            65179
_diffrn_reflns_point_group_measured_fraction_full 0.998
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
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_exptl_crystal_density_diffrn    2.043
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'w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+172.2452P] where P=(Fo^2^+2Fc^2^)/3'
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_cod_data_source_file            Mn6Te6_PMe36.cif
_cod_data_source_block           Mn6Te6-PMe3-6
_cod_original_cell_volume        21287.0(7)
_cod_database_code               4346230
_chemical_oxdiff_formula         'mn6 te6 p6 c18'
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_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.44(6) 0.56(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 P3_1-C4_1 \\sim P3_1-C5_1 \\sim P3_1-C6_1 \\sim P13_1-C14_1 \\sim P13_1-C15_1
\\sim P13_1-C16_1 ~
 P23_1-C24_1 \\sim P23_1-C25_1 \\sim P23_1-C26_1
 P3_2-C4_2 \\sim P3_2-C5_2 \\sim P3_2-C6_2 \\sim P13_2-C14_2 \\sim P13_2-C15_2
\\sim P13_2-C16_2 ~
 P23_2-C24_2 \\sim P23_2-C25_2 \\sim P23_2-C26_2
 P3_3-C4_3 \\sim P3_3-C5_3 \\sim P3_3-C6_3 \\sim P13_3-C14_3 \\sim P13_3-C15_3
\\sim P13_3-C16_3 ~
 P23_3-C24_3 \\sim P23_3-C25_3 \\sim P23_3-C26_3
 P3_4-C4_4 \\sim P3_4-C5_4 \\sim P3_4-C6_4 \\sim P13_4-C14_4 \\sim P13_4-C15_4
\\sim P13_4-C16_4 ~
 P23_4-C24_4 \\sim P23_4-C25_4 \\sim P23_4-C26_4
 with sigma of 0.02
 C4_1-C5_1 \\sim C4_1-C6_1 \\sim C5_1-C6_1 \\sim C14_1-C15_1 \\sim C14_1-C16_1
\\sim C15_1-C16_1 ~
 C24_1-C25_1 \\sim C24_1-C26_1 \\sim C25_1-C26_1
 C4_2-C5_2 \\sim C4_2-C6_2 \\sim C5_2-C6_2 \\sim C14_2-C15_2 \\sim C14_2-C16_2
\\sim C15_2-C16_2 ~
 C24_2-C25_2 \\sim C24_2-C26_2 \\sim C25_2-C26_2
 C4_3-C5_3 \\sim C4_3-C6_3 \\sim C5_3-C6_3 \\sim C14_3-C15_3 \\sim C14_3-C16_3
\\sim C15_3-C16_3 ~
 C24_3-C25_3 \\sim C24_3-C26_3 \\sim C25_3-C26_3
 C4_4-C5_4 \\sim C4_4-C6_4 \\sim C5_4-C6_4 \\sim C14_4-C15_4 \\sim C14_4-C16_4
\\sim C15_4-C16_4 ~
 C24_4-C25_4 \\sim C24_4-C26_4 \\sim C25_4-C26_4
 with sigma of 0.04
 P23_4-Cl92_11 \\sim P23_4-Cl93_11 \\sim P23_1-Cl92_12 \\sim P23_1-Cl93_12
 with sigma of 0.02
 P23_4-C91_11 \\sim P23_1-C91_12
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(Te1_1) = Uanis(Te11_1)
Uanis(Mn2_1) = Uanis(Mn12_1)
Uanis(P3_1) = Uanis(P13_1)
Uanis(C4_1) = Uanis(C14_1)
Uanis(C5_1) = Uanis(C15_1)
Uanis(C6_1) = Uanis(C16_1)
Uanis(Te1_1) = Uanis(Te1_4)
Uanis(Mn2_1) = Uanis(Mn2_4)
Uanis(P3_1) = Uanis(P3_4)
Uanis(C4_1) = Uanis(C4_4)
Uanis(C5_1) = Uanis(C5_4)
Uanis(C6_1) = Uanis(C6_4)
Uanis(Te11_1) = Uanis(Te11_4)
Uanis(Mn12_1) = Uanis(Mn12_4)
Uanis(P13_1) = Uanis(P13_4)
Uanis(C14_1) = Uanis(C14_4)
Uanis(C15_1) = Uanis(C15_4)
Uanis(C16_1) = Uanis(C16_4)
Uanis(Te21_1) = Uanis(Te21_4)
Uanis(Mn22_1) = Uanis(Mn22_4)
Uanis(P23_1) = Uanis(P23_4)
Uanis(C24_1) = Uanis(C24_4)
Uanis(C25_1) = Uanis(C25_4)
Uanis(C26_1) = Uanis(C26_4)
Uanis(Te1_2) = Uanis(Te11_2)
Uanis(Mn2_2) = Uanis(Mn12_2)
Uanis(P3_2) = Uanis(P13_2)
Uanis(C4_2) = Uanis(C14_2)
Uanis(C5_2) = Uanis(C15_2)
Uanis(C6_2) = Uanis(C16_2)
Uanis(Te1_2) = Uanis(Te1_3)
Uanis(Mn2_2) = Uanis(Mn2_3)
Uanis(P3_2) = Uanis(P3_3)
Uanis(C4_2) = Uanis(C4_3)
Uanis(C5_2) = Uanis(C5_3)
Uanis(C6_2) = Uanis(C6_3)
Uanis(Te11_2) = Uanis(Te11_3)
Uanis(Mn12_2) = Uanis(Mn12_3)
Uanis(P13_2) = Uanis(P13_3)
Uanis(C14_2) = Uanis(C14_3)
Uanis(C15_2) = Uanis(C15_3)
Uanis(C16_2) = Uanis(C16_3)
Uanis(Te21_2) = Uanis(Te21_3)
Uanis(Mn22_2) = Uanis(Mn22_3)
Uanis(P23_2) = Uanis(P23_3)
Uanis(C24_2) = Uanis(C24_3)
Uanis(C25_2) = Uanis(C25_3)
Uanis(C26_2) = Uanis(C26_3)
Uanis(Te1_3) = Uanis(Te11_3)
Uanis(Mn2_3) = Uanis(Mn12_3)
Uanis(P3_3) = Uanis(P13_3)
Uanis(C4_3) = Uanis(C14_3)
Uanis(C5_3) = Uanis(C15_3)
Uanis(C6_3) = Uanis(C16_3)
Uanis(Te1_4) = Uanis(Te11_4)
Uanis(Mn2_4) = Uanis(Mn12_4)
Uanis(P3_4) = Uanis(P13_4)
Uanis(C4_4) = Uanis(C14_4)
Uanis(C5_4) = Uanis(C15_4)
Uanis(C6_4) = Uanis(C16_4)
Uanis(C91_11) = Uanis(C91_12)
Uanis(Cl92_11) = Uanis(Cl92_12)
Uanis(Cl93_11) = Uanis(Cl93_12)
5. 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
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{Te1_2, Mn2_2, P3_2, C4_2, C5_2, C6_2, Te11_2, Mn12_2, P13_2, C14_2, C15_2,
C16_2, Te21_2, Mn22_2, P23_2, C24_2, C25_2, C26_2}
{Te1_3, Mn2_3, P3_3, C4_3, C5_3, C6_3, Te11_3, Mn12_3, P13_3, C14_3, C15_3,
C16_3, Te21_3, Mn22_3, P23_3, C24_3, C25_3, C26_3}
{Te1_4, Mn2_4, P3_4, C4_4, C5_4, C6_4, Te11_4, Mn12_4, P13_4, C14_4, C15_4,
C16_4, Te21_4, Mn22_4, P23_4, C24_4, C25_4, C26_4}
as
{Te1_1, Mn2_1, P3_1, C4_1, C5_1, C6_1, Te11_1, Mn12_1, P13_1, C14_1, C15_1,
C16_1, Te21_1, Mn22_1, P23_1, C24_1, C25_1, C26_1} sigma for 1-2: 0.02 1-3: 0.04
7. Others
 Sof(Te1)=Sof(Mn2)=Sof(P3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(Te11)=Sof(Mn12)=
 Sof(P13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(Te21)=Sof(Mn22)=Sof(P23)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(Te1)=Sof(Mn2)=Sof(P3)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(H6C)=Sof(Te11)=Sof(Mn12)=Sof(P13)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(Te21)=Sof(Mn22)=Sof(P23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(Cl92)=Sof(Cl93)=1-FVAR(1)
 Sof(Te1)=Sof(Mn2)=Sof(P3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=
 Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(Te11)=Sof(Mn12)=
 Sof(P13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(Te21)=Sof(Mn22)=Sof(P23)=
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(Te1)=Sof(Mn2)=Sof(P3)=Sof(C4)=
 Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(H6C)=Sof(Te11)=Sof(Mn12)=Sof(P13)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(Te21)=Sof(Mn22)=Sof(P23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=
 Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(Cl92)=Sof(Cl93)=FVAR(1)
8.a Free rotating group:
 C91(Cl92,Cl93), C91(Cl92,Cl93)
8.b Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C91(H91A,H91B)
8.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C4(H4A,H4B,H4C), C5(H5A,H5B,
 H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C4(H4A,
 H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C)
;
_shelx_res_checksum              62945
_shelx_hkl_checksum              73886
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'