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_4129071
_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         'C40 H60 Al Li N4 O3'
_chemical_formula_sum            'C40 H60 Al Li N4 O3'
_chemical_formula_weight         678.84
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-07-11
_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                 93.94(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.944(2)
_cell_length_b                   13.900(3)
_cell_length_c                   25.428(5)
_cell_measurement_reflns_used    2041
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      48
_cell_measurement_theta_min      1.8
_cell_volume                     3859.0(13)
_computing_cell_refinement       'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_computing_data_collection       'COLLECT (Bruker AXS, 1997-2009)'
_computing_data_reduction        'DENZO/SCALEPACK (Bruker AXS, 1997-2009)'
_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 1.000
_diffrn_measurement_device_type  'NONIUS Kappa CCD'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0717
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            13455
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.123
_diffrn_reflns_theta_max         25.123
_diffrn_reflns_theta_min         1.865
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.168
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.264
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6882
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1252
_refine_ls_R_factor_gt           0.0653
_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^)+(0.1126P)^2^+1.1118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1735
_refine_ls_wR_factor_ref         0.2066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3987
_reflns_number_total             6882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10628_si_003.cif
_cod_data_source_block           fe425_3
_cod_original_cell_volume        3859.0(14)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4129071
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.959
_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. Restrained distances
 O51-C51A \\sim O51-C51B \\sim O51-C54A \\sim O51-C54B
 with sigma of 0.02
 C51A-C52A \\sim C52A-C53A \\sim C53A-C54A \\sim C51B-C52B \\sim C52B-C53B
\\sim C53B-C54B
 with sigma of 0.02
 O51-C52A \\sim O51-C53A \\sim O51-C52B \\sim O51-C53B
 with sigma of 0.04
 C52A-C54A \\sim C51A-C53A \\sim C52B-C54B \\sim C51B-C53B
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C51A \\sim C52A \\sim C53A \\sim C54A \\sim
C51B \\sim C52B \\sim C53B \\sim C54B \\sim O31 \\sim O41 \\sim O51: within 1A
with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 O31, C31, C32, C33, C34, O41, C41, C42, C43, C44, O51, C51A, C52A, C53A, C54A,
  C51B, C52B, C53B, C54B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O31, C34, C33, C32, C31} sigma for 1-2: 0.02, 1-3: 0.04
as
{O31, C31, C32, C33, C34}
{O41, C44, C43, C42, C41} sigma for 1-2: 0.02, 1-3: 0.04
as
{O41, C41, C42, C43, C44}
6. Others
 Sof(C51B)=Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C53B)=
 Sof(H53C)=Sof(H53D)=Sof(C54B)=Sof(H54C)=Sof(H54D)=1-FVAR(1)
 Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(C53A)=
 Sof(H53A)=Sof(H53B)=Sof(C54A)=Sof(H54A)=Sof(H54B)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C41(H41A,
 H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C51A(H51A,H51B),
 C52A(H52A,H52B), C53A(H53A,H53B), C54A(H54A,H54B), C51B(H51C,H51D), C52B(H52C,
 H52D), C53B(H53C,H53D), C54B(H54C,H54D)
7.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3A), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C18(H18)
7.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)
;
_shelx_res_checksum              28131
_shelx_hkl_checksum              57089
_olex2_submission_special_instructions 'No special instructions were received'