Spectroscopic Characterization of a Monomeric, Cyclopentadienyl-Based Rhenium(V) Dioxo Complex.
Raju, Suresh; Jastrzebski, Johann T. B. H.; Lutz, Martin; Witteman, Léon; Dethlefsen, Johannes R.; Fristrup, Peter; Moret, Marc-Etienne; Gebbink, Robertus J M Klein; Inorganic chemistry 54 (2015) 11031–11036; doi:10.1021/acs.inorgchem.5b02366

data_4346923
_publ_section_title
;
 Spectroscopic Characterization of a Monomeric, Cyclopentadienyl-Based
 Rhenium(V) Dioxo Complex.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11031
_journal_page_last               11036
_journal_paper_doi               10.1021/acs.inorgchem.5b02366
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C34 H58 O4 Re2'
_chemical_formula_sum            'C34 H58 O4 Re2'
_chemical_formula_weight         903.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                93.955(5)
_cell_angle_beta                 90.787(6)
_cell_angle_gamma                90.472(6)
_cell_formula_units_Z            2
_cell_length_a                   10.3141(12)
_cell_length_b                   11.8978(11)
_cell_length_c                   14.0341(12)
_cell_measurement_reflns_used    15591
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.62
_cell_measurement_theta_min      2.17
_cell_volume                     1717.9(3)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, TWINABS-2012/1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    DIRDIF-08
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.949
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25583
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.724
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    7.074
_exptl_absorpt_correction_T_max  0.43
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS-2012/1
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.13
_refine_diff_density_max         6.204
_refine_diff_density_min         -3.751
_refine_diff_density_rms         0.277
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         7587
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+9.4982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7074
_reflns_number_total             7587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02366_si_002.cif
_cod_data_source_block           l0654a
_cod_database_code               4346923
_shelxl_version_number           2013-4
_shelx_res_checksum              97677
_shelx_hkl_checksum              88826