Synthesis and Characterization of Rhenium(V) Oxo Complexes Bearing PNP-Pincer Ligands
Korstanje, Ties J.; Lutz, Martin; Jastrzebski, Johann T. B. H.; Klein Gebbink, Robertus J. M.; Organometallics 33 (2014) 2201–; doi:10.1021/om401228u

data_4083094
_publ_section_title
;
 Synthesis and Characterization of Rhenium(V) Oxo Complexes Bearing
 PNP-Pincer Ligands
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2201
_journal_paper_doi               10.1021/om401228u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C31 H28 Cl N O2 P2 Re, Cl'
_chemical_formula_sum            'C31 H28 Cl2 N O2 P2 Re'
_chemical_formula_weight         765.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   26.9047(2)
_cell_length_b                   26.9047(2)
_cell_length_c                   23.4468(8)
_cell_measurement_reflns_used    63176
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.51
_cell_volume                     14698.4(5)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2012/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0133
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            75992
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.51
_exptl_absorpt_coefficient_mu    4.009
_exptl_absorpt_correction_T_max  0.7143
_exptl_absorpt_correction_T_min  0.2181
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6768
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.23
_platon_squeeze_details
;
;
_refine_diff_density_max         1.184
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         7511
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0185
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+45.7146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                6793
_reflns_number_total             7511
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om401228u_si_002.cif
_cod_data_source_block           l0289a
_cod_depositor_comments
'Adding full bibliography for 4083093--4083096.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4083094