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_4336154
_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         'C37 H27 B F8 N4 O2 Pd, 0.5(C2 H3 N)'
_chemical_formula_sum            'C38 H28.5 B F8 N4.5 O2 Pd'
_chemical_formula_weight         849.36
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 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                 105.0514(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1584(6)
_cell_length_b                   11.8641(4)
_cell_length_c                   19.9033(7)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.84
_cell_measurement_theta_min      2.21
_cell_volume                     3456.6(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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30380
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.8987
_exptl_absorpt_correction_T_min  0.8577
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       prism
_exptl_crystal_F_000             1708
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.390(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         15822
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0400P)^2^+0.8241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0681
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                14771
_reflns_number_total             15822
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic400911k_si_003.cif
_cod_data_source_block           6c
_cod_original_sg_symbol_H-M      'P c'
_cod_database_code               4336154