Calix[4]arenes of Aluminum and Gallium with Benzimidazolyl Ligands: Steric Control of the Conformation via Substitution on the Ligand
Ernesto Rufino-Felipe; Miguel-Ángel Muñoz-Hernández; Hugo F. Saucedo-Azpeitia; Sara A. Cortes-Llamas; Inorganic Chemistry 51 (2012) 12834–12840; doi:10.1021/ic301718m

data_4331164
_publ_section_title
;
 Calix[4]arenes of Aluminum and Gallium with Benzimidazolyl Ligands:
 Steric Control of the Conformation via Substitution on the Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12834
_journal_page_last               12840
_journal_paper_doi               10.1021/ic301718m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C59 H82 Al4 N7'
_chemical_formula_weight         997.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.446(2)
_cell_angle_beta                 85.244(2)
_cell_angle_gamma                70.262(2)
_cell_formula_units_Z            2
_cell_length_a                   11.2464(17)
_cell_length_b                   14.595(2)
_cell_length_c                   19.441(3)
_cell_measurement_temperature    100(2)
_cell_volume                     2919.9(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22369
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.122
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9725
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_description       block
_exptl_crystal_F_000             1074
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0936
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0716P)^2^+4.6171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                8393
_reflns_number_total             9981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301718m_si_002_3.cif
_cod_data_source_block           Complex_10
_cod_depositor_comments
;

2021-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C118 H164 Al8 N14'
_cod_original_formula_weight         1994.47
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2919.9(8)
_cod_database_code               4331164