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_4078516
_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            'C28.85 H35.74 Br0.04 N3 O Re'
_chemical_formula_weight         629.75
_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                 124.049(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.998(5)
_cell_length_b                   18.682(5)
_cell_length_c                   20.185(7)
_cell_measurement_reflns_used    9300
_cell_measurement_temperature    110
_cell_measurement_theta_max      32.38
_cell_measurement_theta_min      2.50
_cell_volume                     5311(3)
_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 0.987
_diffrn_measured_fraction_theta_max 0.924
_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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            315059
_diffrn_reflns_theta_full        38.09
_diffrn_reflns_theta_max         39.74
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    4.658
_exptl_absorpt_correction_T_max  0.8653
_exptl_absorpt_correction_T_min  0.2505
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       sword
_exptl_crystal_F_000             2513
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         6.324
_refine_diff_density_min         -1.838
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         29933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+8.0442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0677
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                20265
_reflns_number_total             29933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3002872_si_001.cif
_cod_data_source_block           x12066
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4078516