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_4314821
_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(tacn)]'
_chemical_formula_sum            'C6 H15 N3 O3.5 Re'
_chemical_formula_weight         371.41
_chemical_name_common            '[ReO3(tacn)]'
_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                 90.458(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7113(2)
_cell_length_b                   9.9641(4)
_cell_length_c                   15.1570(5)
_cell_measurement_reflns_used    4158
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.9267
_cell_measurement_theta_min      2.4412
_cell_volume                     1013.55(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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0518
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10430
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    11.978
_exptl_absorpt_correction_T_max  0.6458
_exptl_absorpt_correction_T_min  0.4475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2505
_refine_ls_number_restraints     521
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0299
_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^)+(0.0129P)2^+0.0000P] where P=(Fo2^+2Fc2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0382
_refine_ls_wR_factor_ref         0.0415
_reflns_number_gt                1836
_reflns_number_total             2505
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic902114p_si_001_3.cif
_cod_data_source_block           hb17
_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_original_formula_sum        'C6 H15 N3 O3.50 Re'
_cod_database_code               4314821