Propeller-Shaped Aluminum Complexes with an Azaperylene Core in the Ligands
Tsukao, M.; Hashikawa, Y.; Toyama, N.; Muraoka, M.; Murata, M.; Sasamori, T.; Wakamiya, A.; Murata, Y.; Inorganics 7 (2019) 109–; doi:10.3390/inorganics7090109

data_1556431
_publ_section_title
;
 Propeller-Shaped Aluminum Complexes with an Azaperylene Core in the
 Ligands
;
_journal_name_full               Inorganics
_journal_page_first              109
_journal_paper_doi               10.3390/inorganics7090109
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety
'6(C57 H30 Al N3 O3), C0.90 H1.80 Cl1.80, 6(C2 H3 N)'
_chemical_formula_sum            'C354.9 H199.8 Al6 Cl1.8 N24 O18'
_chemical_formula_weight         5313.67
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   34.0652(3)
_cell_length_b                   34.0652(3)
_cell_length_c                   18.1656(2)
_cell_measurement_reflns_used    6965
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      27.499
_cell_measurement_theta_min      2.582
_cell_volume                     18255.9(3)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics
'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      83(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'EIGER X 1M'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.78224
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            68178
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        27.499
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.582
_diffrn_source                   'synchrotron radiation SPring-8 BL40XU'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  1.034
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       needle
_exptl_crystal_F_000             8249
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   1.03425
_exptl_transmission_factor_min   0.97672
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         6965
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0957
_refine_ls_R_factor_gt           0.0791
_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^)+(0.1128P)^2^+30.2208P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2134
_refine_ls_wR_factor_ref         0.2317
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5595
_reflns_number_total             6965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            compoundAl_L3_3.cif
_cod_data_source_block           compoundAl(L3)3
_cod_original_cell_volume        18255.9(4)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C354.90 H199.80 Al6 Cl1.80 N24 O18'
_cod_database_code               1556431
_shelx_estimated_absorpt_t_min   0.997
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              2161
_shelx_hkl_checksum              12361