Calix[4]pyrrole aluminate: a planar tetracoordinate aluminum(III) anion and its unusual Lewis acidity.
Ebner, Fabian; Wadepohl, Hubert; Greb, Lutz; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10628

data_4129068
_publ_section_title
;
 Calix[4]pyrrole aluminate: a planar tetracoordinate aluminum(III) anion
 and its unusual Lewis acidity.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10628
_journal_year                    2019
_chemical_formula_moiety         '1.5(C H2 Cl2), C24 H20 P, C28 H32 Al N4'
_chemical_formula_sum            'C53.5 H55 Al Cl3 N4 P'
_chemical_formula_weight         918.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-17
_audit_creation_method
;
Olex2 1.2
(compiled May 29 2018 13:30:08 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.829(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.455(4)
_cell_length_b                   16.621(3)
_cell_length_c                   23.761(4)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.45
_cell_volume                     9570(3)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.0402
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            184954
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.040
_diffrn_reflns_theta_min         2.052
_diffrn_source                   'microfocus X-ray source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  0.7388
_exptl_absorpt_correction_T_min  0.6851
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1315 before and 0.0700 after correction.
The Ratio of minimum to maximum transmission is 0.9273.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.275
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.792
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         18837
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0601
_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^)+(0.0848P)^2^+15.6945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15023
_reflns_number_total             18837
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10628_si_006.cif
_cod_data_source_block           fe505a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C53.50 H55 Al Cl3 N4 P'
_cod_database_code               4129068
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Cl11, Cl12, Cl21, Cl22, Cl31, Cl32, C91, C91, C93
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Same fragment restrains
{Cl11, Cl12, C91} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl21, Cl22, C92}
{Cl11, Cl12, C91} sigma for 1-2: 0.02, 1-3: 0.04
as
{Cl31, Cl32, C93}
4.a Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B)
4.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106), C108(H108),
 C109(H109), C110(H110), C111(H111), C112(H112), C114(H114), C115(H115),
 C116(H116), C117(H117), C118(H118), C120(H120), C121(H121), C122(H122),
 C123(H123), C124(H124), C202(H202), C203(H203), C204(H204), C205(H205),
 C206(H206), C208(H208), C209(H209), C210(H210), C211(H211), C212(H212),
 C214(H214), C215(H215), C216(H216), C217(H217), C218(H218), C220(H220),
 C221(H221), C222(H222), C223(H223), C224(H224), C2(H2), C3(H3), C7(H7), C8(H8),
  C12(H12), C13(H13), C17(H17), C18(H18), C52(H52), C53(H53), C57(H57),
 C58(H58), C62(H62), C63(H63), C67(H67), C68(H68)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,H73B,H73C),
 C74(H74A,H74B,H74C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C)
;
_shelx_res_checksum              73549
_shelx_hkl_checksum              9697
_olex2_submission_special_instructions 'No special instructions were received'