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_4314820
_publ_section_title
;
 Triazacyclohexane (tach) Complexes of High-Valent Rhenium: Syntheses of
 [(R3tach)ReO3]+ (R = -CH3, -CH2C6H5) and Its Substitution Reactions
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_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(Me3tach)[ReO4]'
_chemical_formula_sum            'C6 H15 N3 O7 Re2'
_chemical_formula_weight         613.61
_chemical_name_common            '[ReO3(Me3tach)[ReO4]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 92.353(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.8270(2)
_cell_length_b                   13.2607(3)
_cell_length_c                   12.9646(3)
_cell_measurement_reflns_used    8102
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      33.6515
_cell_measurement_theta_min      2.5976
_cell_volume                     1344.48(6)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '/o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7445
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    18.019
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.14447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   non
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.963
_refine_diff_density_min         -1.709
_refine_diff_density_rms         0.278
_refine_ls_extinction_coef       0.0045(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc2^\l3^/sin(2\q)]-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2370
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s2^(Fo2^)+(0.0695P)2^+0.0000P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0867
_reflns_number_gt                2157
_reflns_number_total             2370
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902114p_si_001_2.cif
_cod_data_source_block           hb270308
_cod_depositor_comments
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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 
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_cod_database_code               4314820