Synthesis and Characterization of Heterobimetallic (Pd/B) Nindigo Complexes and Comparisons to Their Homobimetallic (Pd2, B2) Analogues
Graeme Nawn; Robert McDonald; Robin G. Hicks; Inorganic Chemistry 52 (2013) 10912–10919; doi:10.1021/ic400911k

data_4336155
_publ_section_title
;
 Synthesis and Characterization of Heterobimetallic (Pd/B) Nindigo
 Complexes and Comparisons to Their Homobimetallic (Pd2, B2) Analogues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10912
_journal_page_last               10919
_journal_paper_doi               10.1021/ic400911k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C45 H43 B F8 N4 O2 Pd, C H2 Cl2'
_chemical_formula_sum            'C46 H45 B Cl2 F8 N4 O2 Pd'
_chemical_formula_weight         1025.97
_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                78.0317(4)
_cell_angle_beta                 88.9814(4)
_cell_angle_gamma                76.9012(4)
_cell_formula_units_Z            2
_cell_length_a                   9.4672(3)
_cell_length_b                   14.2029(5)
_cell_length_c                   17.3360(6)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.37
_cell_volume                     2219.98(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0165
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19880
_diffrn_reflns_theta_full        27.67
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         1.20
_exptl_absorpt_coefficient_mu    0.616
_exptl_absorpt_correction_T_max  0.9461
_exptl_absorpt_correction_T_min  0.8198
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       plate
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.043
_refine_diff_density_min         -1.815
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         10238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+3.4645P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                9195
_reflns_number_total             10238
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic400911k_si_004.cif
_cod_data_source_block           6d
_cod_database_code               4336155