Oxorhenium(V) Complexes with Phenolate-Pyrazole Ligands for Olefin Epoxidation Using Hydrogen Peroxide.
Zwettler, Niklas; Schachner, Jörg A; Belaj, Ferdinand; Mösch-Zanetti, Nadia C; Inorganic chemistry  (2014) 141202093837009–; doi:10.1021/ic501794z

data_4341763
_publ_section_title
;
 Oxorhenium(V) Complexes with Phenolate-Pyrazole Ligands for Olefin
 Epoxidation Using Hydrogen Peroxide.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141202093837009
_journal_paper_doi               10.1021/ic501794z
_journal_year                    2014
_chemical_compound_source        'synthetical product'
_chemical_formula_moiety         'C28 H23 Cl2 N3 O4 P Re'
_chemical_formula_sum            'C28 H23 Cl2 N3 O4 P Re'
_chemical_formula_weight         753.56
_chemical_name_systematic
; dichloro-(2-(1-methylpyrazol-3-yl)-4-nitro-phenolato-N,O)-oxo-(triphenyl-
phosphine)-rhenium(V)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual edited SHELXL-97 .cif file'
_cell_angle_alpha                105.6595(16)
_cell_angle_beta                 99.0462(15)
_cell_angle_gamma                95.7507(16)
_cell_formula_units_Z            2
_cell_length_a                   9.3605(5)
_cell_length_b                   10.4113(5)
_cell_length_c                   14.5555(7)
_cell_measurement_reflns_used    9801
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.73
_cell_measurement_theta_min      2.23
_cell_volume                     1333.60(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25333
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.858
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.517
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0174
_refine_ls_R_factor_gt           0.0164
_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/[\s^2^(Fo^2^)+(0.0189P)^2^+0.9497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0408
_refine_ls_wR_factor_ref         0.0413
_reflns_number_gt                7484
_reflns_number_total             7758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501794z_si_002.cif
_cod_data_source_block           JS17
_cod_database_code               4341763