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_4336153
_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         'C33 H19 B F8 N4 O2 Pd, 0.5(C4 H8 O)'
_chemical_formula_sum            'C35 H23 B F8 N4 O2.5 Pd'
_chemical_formula_weight         808.78
_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                83.4965(8)
_cell_angle_beta                 68.0361(8)
_cell_angle_gamma                64.4777(8)
_cell_formula_units_Z            2
_cell_length_a                   11.3192(8)
_cell_length_b                   12.4363(9)
_cell_length_c                   13.4483(10)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.59
_cell_measurement_theta_min      2.17
_cell_volume                     1581.8(2)
_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    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0217
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14113
_diffrn_reflns_theta_full        27.68
_diffrn_reflns_theta_max         27.68
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.677
_exptl_absorpt_correction_T_max  0.9491
_exptl_absorpt_correction_T_min  0.7309
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.832
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7276
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0600P)^2^+0.8854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1012
_reflns_number_gt                6446
_reflns_number_total             7276
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic400911k_si_002.cif
_cod_data_source_block           6a
_cod_database_code               4336153