Organic Electron Delocalization Modulated by Ligand Charge States in [L<sub>2</sub>M]<sup> <i>n-</i> </sup> Complexes of Group 13 Ions.
Arnold, Amela; Sherbow, Tobias J.; Sayler, Richard I.; Britt, R. David; Thompson, Emily J.; Muñoz, M Teresa; Fettinger, James C.; Berben, Louise A.; Journal of the American Chemical Society 141 (2019) 15792–15803; doi:10.1021/jacs.9b05602

data_4133689
_publ_section_title
;
 Organic Electron Delocalization Modulated by Ligand Charge States in
 [L<sub>2</sub>M]<sup> <i>n-</i> </sup> Complexes of Group 13 Ions.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15792
_journal_page_last               15803
_journal_paper_doi               10.1021/jacs.9b05602
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C66 H54 Al N6 O4 [+ solvent]'
_chemical_formula_sum            'C66 H54 Al N6 O4'
_chemical_formula_weight         1022.13
_space_group_crystal_system      tetragonal
_space_group_IT_number           76
_space_group_name_Hall           'P 4w'
_space_group_name_H-M_alt        'P 41'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5799(3)
_cell_length_b                   13.5799(3)
_cell_length_c                   37.5593(7)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      72.05
_cell_measurement_theta_min      3.25
_cell_volume                     6926.4(3)
_computing_cell_refinement       'SAINT (8.37a) (Bruker, 2016)'
_computing_data_collection       'Apex3 (2017.3) (Bruker, 2017)'
_computing_data_reduction        'SAINT (8.37a) (Bruker, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0459
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            22947
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.136
_diffrn_reflns_theta_min         3.254
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_T_max  0.8890
_exptl_absorpt_correction_T_min  0.7654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Sheldrick, 2016)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    0.980
_exptl_crystal_description       Block
_exptl_crystal_F_000             2148
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.184
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.18(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     699
_refine_ls_number_reflns         12644
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0680P)^2^+0.4517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1182
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_full    0.988
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                11551
_reflns_number_total             12644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05602_si_001.cif
_cod_data_source_block           TJS77FMI_SQ
_cod_depositor_comments
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The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4133689
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              59615
_shelx_hkl_checksum              26527
_shelx_fab_checksum              93996