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_4083093
_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         'C49 H42 N O2 P3 Re, I'
_chemical_formula_sum            'C49 H42 I N O2 P3 Re'
_chemical_formula_weight         1082.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.7636(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9296(4)
_cell_length_b                   30.5378(9)
_cell_length_c                   13.9871(5)
_cell_measurement_reflns_used    9934
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.30
_cell_volume                     4644.8(3)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       Apex2
_computing_data_reduction        'SAINT V7.68A, SADABS-2008/1, SQUEEZE'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            54399
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    3.422
_exptl_absorpt_correction_T_max  0.4305
_exptl_absorpt_correction_T_min  0.3366
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
;
_refine_diff_density_max         1.603
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         10631
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+1.6065P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                8514
_reflns_number_total             10631
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om401228u_si_002.cif
_cod_data_source_block           l0265a
_cod_depositor_comments
'Adding full bibliography for 4083093--4083096.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4083093