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_4346924
_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         'C19 H33 O3 Re'
_chemical_formula_sum            'C19 H33 O3 Re'
_chemical_formula_weight         495.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 97.5339(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9274(3)
_cell_length_b                   18.1800(7)
_cell_length_c                   12.1650(4)
_cell_measurement_reflns_used    9661
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.30
_cell_volume                     1957.34(12)
_computing_cell_refinement       'SAINT V8.27B'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V8.27B, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0114
_diffrn_reflns_av_unetI/netI     0.0077
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            23815
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.561
_diffrn_reflns_theta_min         2.026
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.220
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.153
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         4522
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0142
_refine_ls_R_factor_gt           0.0138
_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^)+(0.0082P)^2^+2.7365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0309
_refine_ls_wR_factor_ref         0.0310
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4441
_reflns_number_total             4522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02366_si_002.cif
_cod_data_source_block           l0652a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4346924
_shelxl_version_number           2013-4
_shelx_res_checksum              92559
_shelx_hkl_checksum              73466