Mono- and Bis- Methyltrioxorhenium(VII) Complexes with Salen Ligands: Synthesis, Properties, Applications
Zhaoqing Xu; Ming-Dong Zhou; Markus Drees; Hugh Chaffey-Millar; Eberhardt Herdtweck; Wolfgang A. Herrmann; Fritz E. Kühn; Inorganic Chemistry 48 (2009) 6812–6822; doi:10.1021/ic900761u

data_4302749
_publ_contact_author_address
;
       Department Chemie,
       Lehrstuhl f\"ur Anorganische Chemie,
       Technische Universit\"at M\"unchen,
       Lichtenbergstrasse 4,
       D-85747 Garching bei M\"unchen,
       Germany.
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         '+49(0)89 289 13473'
_publ_contact_author_name
;
       Dr. Eberhardt Herdtweck
;
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
Mono- and Bis- Methyltrioxorhenium(VII) Complexes with Salen Ligands:
Synthesis, Properties, Applications
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6812
_journal_page_last               6822
_journal_paper_doi               10.1021/ic900761u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C24 H32 N2 O10 Re2'
_chemical_formula_sum            'C24 H32 N2 O10 Re2'
_chemical_formula_weight         880.94
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 115.555(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.8092(9)
_cell_length_b                   12.6315(6)
_cell_length_c                   12.9568(6)
_cell_measurement_reflns_used    27236
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      4.75
_cell_volume                     2777.2(2)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-AREA (Stoe, 2004)'
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR92 (Altomare, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 'image plate'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'IPDS 2T (Stoe)'
_diffrn_measurement_method       'omega-rotation/oscillation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'NONIUS FR 591 rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_sigmaI/netI    0.0154
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20762
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         4.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    8.766
_exptl_absorpt_correction_T_max  0.4016
_exptl_absorpt_correction_T_min  0.1209
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 Numerical absorption correction after crystal shape optimization
 source: (Stoe, 2004)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.107
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       column
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.464
_refine_diff_density_rms         0.087
_refine_ls_extinction_coef       0.00055(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         2530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_gt           0.0201
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+3.6701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0456
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                2235
_reflns_number_total             2530
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic900761u_si_002_2.cif
_cod_data_source_block           Compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4302749