Synthesis, structures, redox properties, and theoretical calculations of thiohalide capped octahedral hexanuclear technetium(iii) clusters.
Yoshimura, Takashi; Nagata, Kojiro; Matsuda, Ayumi; Omote, Toshiki; Kino, Yasushi; Takayama, Tsutomu; Sekine, Tsutomu; Shinohara, Atsushi; Dalton transactions (Cambridge, England : 2003) 48 (2019) 14085–14095; doi:10.1039/c9dt02909e

data_7701599
_publ_section_title
;
 Synthesis, structures, redox properties, and theoretical calculations of
 thiohalide capped octahedral hexanuclear technetium(iii) clusters.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14085
_journal_page_last               14095
_journal_paper_doi               10.1039/c9dt02909e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(Br3.5 S3.5 Tc3), 3(C24 H20 P)'
_chemical_formula_sum            'C72 H60 Br7 P3 S7 Tc6'
_chemical_formula_weight         2395.29
_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             2019-05-13
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-15 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                92.4670(10)
_cell_angle_beta                 108.9090(10)
_cell_angle_gamma                100.7220(10)
_cell_formula_units_Z            2
_cell_length_a                   13.8962(4)
_cell_length_b                   15.1967(4)
_cell_length_c                   19.6412(7)
_cell_measurement_reflns_used    28192
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     3831.5(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  RAPID
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0860
_diffrn_reflns_av_unetI/netI     0.1080
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37485
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.047
_exptl_absorpt_coefficient_mu    4.997
_exptl_absorpt_correction_T_max  0.607
_exptl_absorpt_correction_T_min  0.193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_description       plate
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.553
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     864
_refine_ls_number_reflns         17274
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0504
_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^)+(0.0226P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12022
_reflns_number_total             17274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02909e2.cif
_cod_data_source_block           PPh4[Tc6S7Br7]
_cod_database_code               7701599
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Br21, S21}
{Br23, S23}
{Br22, S22}
{Br24, S24}
{Br11, S11}
{Br12, S12}
{Br13, S13}
{Br14, S14}
3. Uiso/Uaniso restraints and constraints
Uanis(Br21) = Uanis(S21)
Uanis(Br23) = Uanis(S23)
Uanis(Br22) = Uanis(S22)
Uanis(Br24) = Uanis(S24)
Uanis(Br11) = Uanis(S11)
Uanis(Br12) = Uanis(S12)
Uanis(Br13) = Uanis(S13)
Uanis(Br14) = Uanis(S14)
4. Others
 1*[Sof(Br21)+Sof(S21)]+1*[Sof(Br23)+Sof(S23)]+1*[Sof(Br22)+Sof(S22)]+1*
 [Sof(Br24)+Sof(S24)]=0.5 with esd of 0.0001
 1*[Sof(Br11)+Sof(S11)]+1*[Sof(Br12)+Sof(S12)]+1*[Sof(Br13)+Sof(S13)]+1*
 [Sof(Br14)+Sof(S14)]=0.5 with esd of 0.0001
 Sof(S21)=1-FVAR(1)
 Sof(Br21)=FVAR(1)
 Sof(S23)=1-FVAR(2)
 Sof(Br23)=FVAR(2)
 Sof(S22)=1-FVAR(3)
 Sof(Br22)=FVAR(3)
 Sof(S24)=1-FVAR(4)
 Sof(Br24)=FVAR(4)
 Sof(S11)=1-FVAR(5)
 Sof(Br11)=FVAR(5)
 Sof(S12)=1-FVAR(6)
 Sof(Br12)=FVAR(6)
 Sof(S13)=1-FVAR(7)
 Sof(Br13)=FVAR(7)
 Sof(S14)=1-FVAR(8)
 Sof(Br14)=FVAR(8)
5.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C29(H29),
 C30(H30), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39),
  C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57),
  C58(H58), C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65),
 C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
;
_olex2_submission_special_instructions 'No special instructions were received'