Synthesis of Cyclopentadienyl-Based Trioxo-rhenium Complexes and Their Use as Deoxydehydration Catalysts
Raju, Suresh; van Slagmaat, Christian A. M. R.; Li, Jing; Lutz, Martin; Jastrzebski, Johann T. B. H.; Moret, Marc-Etienne; Klein Gebbink, Robertus J. M.; Organometallics 35 (2016) 2178–; doi:10.1021/acs.organomet.6b00120

data_4086547
_publ_section_title
;
 Synthesis of Cyclopentadienyl-Based Trioxo-rhenium Complexes and Their
 Use as Deoxydehydration Catalysts
;
_journal_issue                   13
_journal_name_full               Organometallics
_journal_page_first              2178
_journal_paper_doi               10.1021/acs.organomet.6b00120
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C9 H13 O3 Re'
_chemical_formula_sum            'C9 H13 O3 Re'
_chemical_formula_weight         355.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.9964(3)
_cell_length_b                   13.1856(7)
_cell_length_c                   12.0268(7)
_cell_measurement_reflns_used    5125
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      3.09
_cell_volume                     950.91(9)
_computing_cell_refinement       'SAINT V8.27B'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V8.27B, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13014
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    12.749
_exptl_absorpt_correction_T_max  0.4326
_exptl_absorpt_correction_T_min  0.3162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.130
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0251
_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
'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+0.9589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0416
_refine_ls_wR_factor_ref         0.0434
_reflns_number_gt                1280
_reflns_number_total             1452
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6b00120_si_002.cif
_cod_data_source_block           l0436b
_cod_depositor_comments
'Adding full bibliography for 4086544--4086547.cif.'
_cod_database_code               4086547