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_4083096
_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 H51 Cl2 N O P2 Re, O4 Re'
_chemical_formula_sum            'C31 H51 Cl2 N O5 P2 Re2'
_chemical_formula_weight         1022.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.283(3)
_cell_angle_beta                 87.606(3)
_cell_angle_gamma                80.396(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7444(6)
_cell_length_b                   10.9303(7)
_cell_length_c                   16.9114(8)
_cell_measurement_reflns_used    21428
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.92
_cell_volume                     1750.32(18)
_computing_cell_refinement       Peakref
_computing_data_collection       Apex2
_computing_data_reduction        'Eval15, SADABS-2008/1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32871
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    7.193
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.2631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.460
_refine_diff_density_min         -1.178
_refine_diff_density_rms         0.190
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8025
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0409
_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^)+(0.0477P)^2^+6.5324P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                6113
_reflns_number_total             8025
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om401228u_si_002.cif
_cod_data_source_block           l0328a
_cod_depositor_comments
'Adding full bibliography for 4083093--4083096.cif.'
_cod_original_cell_volume        1750.33(17)
_cod_database_code               4083096