Bidentate Lewis Base Adducts of Methyltrioxorhenium(VII) and Their Application in Catalytic Epoxidation
Paula Ferreira; Wen-Mei Xue; Éva Bencze; Eberhardt Herdtweck; Fritz E. Kühn; Inorganic Chemistry 40 (2001) 5834–5841; doi:10.1021/ic010610f

data_4320542
_publ_contact_author
;
         Dr. Eberhardt Herdtweck
         Anorganisch-chemisches Institut der
         Technischen Universit\"at M\"unchen
         Lichtenbergstrasse 4
         D-85747 Garching bei M\"unchen
;
_publ_contact_author_email       eberhardt.herdtweck@ch.tum.de
_publ_contact_author_fax         ' +49(0)89 289 13473'
_publ_contact_author_phone       '+49(0)89 289 13143'
_publ_section_title
;
 Bidentate Lewis Base Adducts of Methyltrioxorhenium(VII) and Their
 Application in Catalytic Epoxidation
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5834
_journal_page_last               5841
_journal_paper_doi               10.1021/ic010610f
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C13 H11 N2 O3 Re'
_chemical_formula_sum            'C13 H11 N2 O3 Re'
_chemical_formula_weight         429.45
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             22-Jan-01
_audit_creation_method           'PLATON <TABLE ACC> option'
_audit_update_record
;
   14-Feb-01  Updated by the Author E.H.
   1-Jun-01  Updated by the Author E.H.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.2269(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6152(1)
_cell_length_b                   11.6056(2)
_cell_length_c                   12.7074(2)
_cell_measurement_reflns_used    2914
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.42
_cell_volume                     1219.93(3)
_computing_cell_refinement       'Denzo and HKL (Nonius, 2001)'
_computing_data_collection       'Kappa CCD (Nonius, 2000)'
_computing_data_reduction        'Denzo and HKL (Nonius,2001)'
_computing_molecular_graphics    'PLATON PLUTON (Spek, 2000)'
_computing_publication_material  'PLATON (Spek, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Kappa CCD (Nonius)'
_diffrn_measurement_method       ' phi- and omega-rotation '
_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  0.037
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21079
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    9.966
_exptl_absorpt_correction_T_max  0.091
_exptl_absorpt_correction_T_min  0.031
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   Denzo-SNM; Scale-Pack
.absorption correction done during scaling
;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.338
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       fragment
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.937
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0058(2)
_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   1.108
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0189
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+4.2796P]   where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0439
_refine_ls_wR_factor_ref         0.0443
_reflns_number_gt                2693
_reflns_number_total             2794
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic010610f.cif
_cod_data_source_block           WANH-4107-173
_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.

'_exptl_absorpt_correction_type' value 'multi scan'
changed to 'multi-scan' 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 

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      'P 21/n'
_cod_database_code               4320542