Triazacyclohexane (tach) Complexes of High-Valent Rhenium: Syntheses of [(R3tach)ReO3]+ (R = -CH3, -CH2C6H5) and Its Substitution Reactions
Henrik Braband; Sebastian Imstepf; Michael Felber; Bernhard Spingler; Roger Alberto; Inorganic Chemistry 49 (2010) 1283–1285; doi:10.1021/ic902114p

data_4314819
_publ_section_title
;
 Triazacyclohexane (tach) Complexes of High-Valent Rhenium: Syntheses of
 [(R3tach)ReO3]+ (R = -CH3, -CH2C6H5) and Its Substitution Reactions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1283
_journal_page_last               1285
_journal_paper_doi               10.1021/ic902114p
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         '[ReO3(Bn3tach)][ReO4]'
_chemical_formula_sum            'C88 H113 N9 O25 Re6'
_chemical_formula_weight         2814.07
_chemical_name_common            '[ReO3(Bn3tach)][ReO4]'
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 117.178(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6742(5)
_cell_length_b                   27.0169(5)
_cell_length_c                   20.3448(4)
_cell_measurement_reflns_used    16554
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.4348
_cell_measurement_theta_min      2.4638
_cell_volume                     9620.0(4)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_sigmaI/netI    0.2155
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            104940
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    7.595
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.943
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5416
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.474
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.722
_refine_ls_hydrogen_treatment    constrains
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         21695
_refine_ls_number_restraints     191
_refine_ls_restrained_S_all      0.724
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0084P)2^+0.0000P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0495
_reflns_number_gt                9395
_reflns_number_total             21695
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902114p_si_001_1.cif
_cod_data_source_block           ssi_210909
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4314819