Bis-Metal Complexes of Doubly N-Confused Dioxohexaphyrins as Potential Near Infrared-II Photoacoustic Dyes.
Shimomura, Keito; Kai, Hiroto; Nakamura, Yuma; Hong, Yongseok; Mori, Shigeki; Miki, Koji; Ohe, Kouichi; Notsuka, Yusuke; Yamaoka, Yoshihisa; Ishida, Masatoshi; Kim, Dongho; Furuta, Hiroyuki; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b13475

data_4134202
_publ_section_title
;
 Bis-Metal Complexes of Doubly N-Confused Dioxohexaphyrins as Potential
 Near Infrared-II Photoacoustic Dyes.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b13475
_journal_year                    2020
_chemical_formula_moiety         'C66 H10 Cu2 F30 N6 O2, 2(C H2 Cl2)'
_chemical_formula_sum            'C68 H14 Cl4 Cu2 F30 N6 O2'
_chemical_formula_weight         1785.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 97.891(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4761(5)
_cell_length_b                   25.9270(9)
_cell_length_c                   25.4632(9)
_cell_measurement_reflns_used    13762
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.14
_cell_measurement_theta_min      2.24
_cell_volume                     6196.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_publication_material  'CrystalStructure 4.2.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            50539
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         1.615
_diffrn_source                   'Varimax 50 kV 24 mA Rotating anode'
_exptl_absorpt_coefficient_mu    1.006
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.880
_refine_diff_density_min         -1.185
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         7114
_refine_ls_number_restraints     840
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.1302
_refine_ls_R_factor_gt           0.0986
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2325
_refine_ls_wR_factor_ref         0.2485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5177
_reflns_number_total             7114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b13475_si_004.cif
_cod_data_source_block           shelxl
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               4134202
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              75954
_shelx_hkl_checksum              11957