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_7701600
_publ_section_title
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 Synthesis, structures, redox properties, and theoretical calculations of
 thiohalide capped octahedral hexanuclear technetium(iii) clusters.
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_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         'Br8 S6 Tc6, 2(C24 H20 P), C H4 O'
_chemical_formula_sum            'C49 H44 Br8 O P2 S6 Tc6'
_chemical_formula_weight         2135.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-05-13
_audit_creation_method
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Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2019-07-15 deposited with the CCDC.	2019-09-06 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 93.548(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.161(3)
_cell_length_b                   21.436(6)
_cell_length_c                   14.254(4)
_cell_measurement_reflns_used    17735
_cell_measurement_temperature    170
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.02
_cell_volume                     3098.7(15)
_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 0.998
_diffrn_measured_fraction_theta_max 0.994
_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  0.000
_diffrn_reflns_av_unetI/netI     0.1242
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7057
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.444
_diffrn_reflns_theta_min         3.017
_exptl_absorpt_coefficient_mu    6.748
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.3520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.289
_exptl_crystal_description       block
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.119
_refine_diff_density_min         -2.329
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.901
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1034
_refine_ls_wR_factor_ref         0.1185
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4367
_reflns_number_total             7057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02909e2.cif
_cod_data_source_block           (PPh4)2[Tc6S6Br8]
_cod_database_code               7701600
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Shared sites
{Br12, S12}
{S13, Br13}
{Br11, S11}
{Br14, S14}
3. Restrained distances
 C25-O1
 1.5 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Br12) = Uanis(S12)
Uanis(S13) = Uanis(Br13)
Uanis(Br11) = Uanis(S11)
Uanis(Br14) = Uanis(S14)
5. Others
 1*[Sof(S12)+Sof(Br12)]+1*[Sof(S13)+Sof(Br13)]+1*[Sof(S11)+Sof(Br11)]+1*
 [Sof(S14)+Sof(Br14)]=1 with esd of 0.0001
 Sof(S12)=1-FVAR(1)
 Sof(Br12)=FVAR(1)
 Sof(S13)=1-FVAR(2)
 Sof(Br13)=FVAR(2)
 Sof(S11)=1-FVAR(3)
 Sof(Br11)=FVAR(3)
 Sof(S14)=1-FVAR(4)
 Sof(Br14)=FVAR(4)
 Fixed Sof: O1(0.5) H1(0.5) C25(0.5) H25A(0.5) H25B(0.5) H25C(0.5)
6.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)
6.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
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_olex2_submission_special_instructions 'No special instructions were received'