Palladacycles Based on 8-Aminoquinoline Carboxamides of Cobalt and Iron Sandwich Compounds and a New Method to α-Alkylate Cp Rings of Metal Sandwich Carboxamides
Singh, Jatinder; Deb, Mayukh; Elias, Anil J.; Organometallics 34 (2015) 4946–; doi:10.1021/acs.organomet.5b00504

data_4087693
_publ_section_title
;
 Palladacycles Based on 8-Aminoquinoline Carboxamides of Cobalt and Iron
 Sandwich Compounds and a New Method to \a-Alkylate Cp Rings of Metal
 Sandwich Carboxamides
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4946
_journal_paper_doi               10.1021/acs.organomet.5b00504
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C45 H32 Co N3 O Pd'
_chemical_formula_sum            'C45 H32 Co N3 O Pd'
_chemical_formula_weight         796.07
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                105.394(4)
_cell_angle_beta                 94.066(4)
_cell_angle_gamma                98.241(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4178(18)
_cell_length_b                   11.198(2)
_cell_length_c                   19.541(4)
_cell_measurement_temperature    298(2)
_cell_volume                     1953.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0966
_diffrn_reflns_av_sigmaI/netI    0.1325
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19093
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808.0
_exptl_crystal_size_max          0.297
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.117
_platon_squeeze_details
;
;
_refine_diff_density_max         0.695
_refine_diff_density_min         -1.604
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1199
_refine_ls_R_factor_gt           0.0809
_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^)+(0.0864P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1825
_refine_ls_wR_factor_ref         0.1969
_reflns_number_gt                4643
_reflns_number_total             6878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00504_si_002.cif
_cod_data_source_block           3
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4087693