Hetero Cu(III)-Pd(II) Complex of a Dibenzo[g,p]chrysene-Fused Bis-dicarbacorrole with Stable Organic Radical Character.
Ke, Xian-Sheng; Hong, Yongseok; Tu, Peiyu; He, Qing; Lynch, Vincent M.; Kim, Dongho; Sessler, Jonathan L.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09167

data_4126589
_publ_section_title
;
 Hetero Cu(III)-Pd(II) Complex of a Dibenzo[g,p]chrysene-Fused
 Bis-dicarbacorrole with Stable Organic Radical Character.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09167
_journal_year                    2017
_chemical_formula_moiety         'C96 H60 N4 F10, Cu, Pd'
_chemical_formula_sum            'C96 H60 Cu F10 N4 Pd'
_chemical_formula_weight         1629.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 94.853(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.622(6)
_cell_length_b                   12.955(3)
_cell_length_c                   32.433(7)
_cell_measurement_reflns_used    19654
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.00
_cell_volume                     10727(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;

Sir2004.  Burla M.C., Caliandro, R., Camalli M., Carrozzini, B., Cascarano G.L., 
De Caro, L., Giacovazzo C., Polidori G., Spagna R. 
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_unetI/netI     0.1920
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35839
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.028
_diffrn_reflns_theta_min         1.849
_diffrn_source                   'sealed fine focus tube'
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.563
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.009
_exptl_crystal_description       block
_exptl_crystal_F_000             3316
_exptl_crystal_size_max          0.107
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1115
_refine_ls_number_reflns         18761
_refine_ls_number_restraints     1003
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1759
_refine_ls_R_factor_gt           0.1108
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1043P)^2^+0.8893P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2410
_refine_ls_wR_factor_ref         0.2908
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9745
_reflns_number_total             18761
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09167_si_004.cif
_cod_data_source_block           shelx
_cod_database_code               4126589
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              32554
_shelx_hkl_checksum              93777
_shelx_fab_checksum              31393