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_4126591
_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 -4, 2 Cu 2+'
_chemical_formula_sum            'C96 H60 Cu2 F10 N4'
_chemical_formula_weight         1586.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 99.589(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.6091(5)
_cell_length_b                   12.3660(3)
_cell_length_c                   17.1126(4)
_cell_measurement_reflns_used    9477
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5
_cell_measurement_theta_min      3.58
_cell_volume                     4508.91(19)
_computing_cell_refinement
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_collection
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2016/6, Sheldrick, G. M.'
_computing_structure_solution
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Agilent SuperNova with Atlas S2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25144
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.972
_diffrn_reflns_theta_min         3.574
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       plate
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.340
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.956
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.084
_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     511
_refine_ls_number_reflns         9139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1235P)^2^+2.9025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6389
_reflns_number_total             9139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09167_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4126591
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.702
_shelx_estimated_absorpt_t_max   0.936
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              4903
_shelx_hkl_checksum              39850
_shelx_fab_checksum              6195