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_4126590
_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 H66 F10 N4'
_chemical_formula_sum            'C96 H66 F10 N4'
_chemical_formula_weight         1465.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 123.12(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.296(7)
_cell_length_b                   12.4764(12)
_cell_length_c                   27.728(4)
_cell_measurement_reflns_used    1060
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.5
_cell_measurement_theta_min      3.51
_cell_volume                     8488(3)
_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-2013, 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 0.992
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0903
_diffrn_reflns_av_unetI/netI     0.1235
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            15763
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.252
_diffrn_reflns_theta_min         3.533
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_description       plate
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.412
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8207
_refine_ls_number_restraints     330
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1850
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1209P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2238
_refine_ls_wR_factor_ref         0.2937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3529
_reflns_number_total             8207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09167_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               4126590
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              77174
_shelx_hkl_checksum              80973
_shelx_fab_checksum              3103