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_4086544
_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         'C13 H21 O3 Re'
_chemical_formula_sum            'C13 H21 O3 Re'
_chemical_formula_weight         411.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 118.867(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.3051(3)
_cell_length_b                   19.3260(14)
_cell_length_c                   6.3244(5)
_cell_measurement_reflns_used    5008
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      3.69
_cell_volume                     674.89(8)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, Platon-ABST, mergehklf5'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    DIRDIF-08
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker Kappa ApexII'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10858
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.780
_diffrn_reflns_theta_min         2.108
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    8.997
_exptl_absorpt_correction_T_max  0.687
_exptl_absorpt_correction_T_min  0.076
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   Platon-ABST
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.025
_exptl_crystal_description       plate
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.733
_refine_diff_density_min         -1.487
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+4.5575P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0649
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1983
_reflns_number_total             1992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00120_si_002.cif
_cod_data_source_block           l0676a
_cod_depositor_comments
'Adding full bibliography for 4086544--4086547.cif.'
_cod_original_cell_volume        674.88(8)
_cod_database_code               4086544
_shelxl_version_number           2013-4
_shelx_res_checksum              43634
_shelx_hkl_checksum              31433