Synthesis of Oxorhenium Acetyl and Benzoyl Complexes Incorporating Diamidopyridine Ligands: Implications for the Mechanism of CO Insertion
Lilly, Cassandra P.; Boyle, Paul D.; Ison, Elon A.; Organometallics 31 (2012) 4295–; doi:10.1021/om3002872

data_4078515
_publ_section_title
;
 Synthesis of Oxorhenium Acetyl and Benzoyl Complexes Incorporating
 Diamidopyridine Ligands: Implications for the Mechanism of CO Insertion
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              4295
_journal_paper_doi               10.1021/om3002872
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C32 H34 N3 O2 Re'
_chemical_formula_weight         678.82
_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                78.110(18)
_cell_angle_beta                 79.25(2)
_cell_angle_gamma                75.795(18)
_cell_formula_units_Z            4
_cell_length_a                   13.536(5)
_cell_length_b                   13.995(4)
_cell_length_c                   15.660(6)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    110
_cell_measurement_theta_max      31.74
_cell_measurement_theta_min      2.90
_cell_volume                     2785.1(17)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    XS
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.643
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Axis X8 Apex2'
_diffrn_measurement_method       'omega and phi 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  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            55668
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         32.31
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    4.397
_exptl_absorpt_correction_T_max  0.9532
_exptl_absorpt_correction_T_min  0.7117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.928
_refine_diff_density_min         -1.501
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     697
_refine_ls_number_reflns         12757
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0334P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                8428
_reflns_number_total             12757
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3002872_si_001.cif
_cod_data_source_block           x12052
_cod_original_cell_volume        2785.0(17)
_cod_database_code               4078515