Synthesis and Properties of meso-Arylated Corrphycenes.
Nozawa, Ryo; Shinokubo, Hiroshi; Organic letters 19 (2017) 4928–4931; doi:10.1021/acs.orglett.7b02390

data_1547581
_publ_section_title
;
 Synthesis and Properties of meso-Arylated Corrphycenes.
;
_journal_issue                   18
_journal_name_full               'Organic letters'
_journal_page_first              4928
_journal_page_last               4931
_journal_paper_doi               10.1021/acs.orglett.7b02390
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C51 H42 Cl2 N4 Pd'
_chemical_formula_weight         888.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.308(8)
_cell_length_b                   15.883(10)
_cell_length_c                   19.472(13)
_cell_measurement_reflns_used    4411
_cell_measurement_temperature    109
_cell_measurement_theta_max      27.2933
_cell_measurement_theta_min      2.2514
_cell_volume                     4116(5)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      109
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  Imus
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47361
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.475
_diffrn_reflns_theta_min         2.092
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_description       prism
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.330
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.367
_refine_diff_density_min         -1.141
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.913
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         8407
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.084
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.814
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.941
_reflns_number_gt                7885
_reflns_number_total             8407
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02390_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               1547581
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              37994
_shelx_hkl_checksum              68554