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_4078514
_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            'C31 H34 N3 O Re'
_chemical_formula_weight         650.81
_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                 92.891(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.067(6)
_cell_length_b                   16.635(7)
_cell_length_c                   18.941(7)
_cell_measurement_reflns_used    9482
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.64
_cell_measurement_theta_min      2.45
_cell_volume                     5371(4)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0512
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            268665
_diffrn_reflns_theta_full        37.83
_diffrn_reflns_theta_max         37.83
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    4.553
_exptl_absorpt_correction_T_max  0.5890
_exptl_absorpt_correction_T_min  0.4767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.171
_refine_diff_density_min         -1.256
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         28528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+2.2206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                19824
_reflns_number_total             28528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3002872_si_001.cif
_cod_data_source_block           x12037
_cod_original_cell_volume        5371(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078514