Aromaticity switching via azulene transformations in azulene-bridged A,D-dithiahexaphyrin.
Białek, Michał J; Latos-Grażyński, Lechosław; Chemical communications (Cambridge, England) 54 (2018) 1837–1840; doi:10.1039/c7cc08754c

data_7121017
_publ_section_title
;
 Aromaticity switching via azulene transformations in azulene-bridged
 A,D-dithiahexaphyrin.
;
_journal_issue                   15
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1837
_journal_page_last               1840
_journal_paper_doi               10.1039/c7cc08754c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C82 H44 D16 N4 O Pd S2'
_chemical_formula_weight         1303.95
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-01 deposited with the CCDC.
2017-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                106.13(3)
_cell_angle_beta                 93.46(2)
_cell_angle_gamma                90.79(2)
_cell_formula_units_Z            2
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_cell_length_b                   16.969(3)
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_cell_measurement_reflns_used    1656
_cell_measurement_temperature    79.9(6)
_cell_measurement_theta_max      23.0490
_cell_measurement_theta_min      3.0330
_cell_volume                     3286.2(11)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      79.9(6)
_diffrn_detector_area_resol_mean 10.3456
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1539
_diffrn_reflns_av_unetI/netI     0.3716
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26208
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.748
_exptl_absorpt_coefficient_mu    0.397
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_description       needle
_exptl_crystal_F_000             1332
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: deuterated toluene'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.653
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     817
_refine_ls_number_reflns         12892
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.966
_refine_ls_R_factor_all          0.2224
_refine_ls_R_factor_gt           0.0883
_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^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.2101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5184
_reflns_number_total             12892
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08754c2.cif
_cod_data_source_block           PdSNaph
_cod_depositor_comments
'Adding full bibliography for 7121016--7121017.cif.'
_cod_database_code               7121017
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.925
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_shelx_res_checksum              87521
_shelx_fab_checksum              89887