Diverse reactivity of an Al(I)-centred anion towards ketones.
Liu, Han-Ying; Hill, Michael S.; Mahon, Mary F.; Chemical communications (Cambridge, England)  (2022) –; doi:10.1039/d2cc02333d

data_7130186
_publ_section_title
;
 Diverse reactivity of an Al(I)-centred anion towards ketones.
;
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d2cc02333d
_journal_year                    2022
_chemical_formula_moiety         '0.25(C156 H272 Al4 K4 N8 O4 Si8)'
_chemical_formula_sum            'C39 H68 Al K N2 O Si2'
_chemical_formula_weight         703.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-06
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-19 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 127.202(3)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   44.6873(10)
_cell_length_b                   12.43270(10)
_cell_length_c                   37.5655(8)
_cell_measurement_reflns_used    33906
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.6520
_cell_measurement_theta_min      4.2810
_cell_volume                     16623.8(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       55
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            156548
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.284
_diffrn_reflns_theta_min         3.761
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.094
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       block
_exptl_crystal_F_000             6144
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.596
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1030
_refine_ls_number_reflns         16566
_refine_ls_number_restraints     499
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+15.9834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1066
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14031
_reflns_number_total             16566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02333d2.cif
_cod_data_source_block           s22msh26-cpd14
_cod_original_cell_volume        16623.8(7)
_cod_database_code               7130186
_shelxl_version_number           2014-3
_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. Restrained distances
 C39-C36 \\sim C39A-C36 \\sim C37-C36 \\sim C37A-C36 \\sim C38-C36 \\sim
C38A-C36
 with sigma of 0.005
 C11A-C10A \\sim C11-C10 \\sim C12-C10 \\sim C12A-C10A \\sim C8A-C7A \\sim
C8-C7 \\sim C9A-C7A \\sim C9-C7
 with sigma of 0.005
 C7-C2 \\sim C7A-C2A \\sim C6A-C10A \\sim C6-C10
 with sigma of 0.005
 C37-C37A \\sim C38-C38A \\sim C39-C39A
 with sigma of 0.02
 C39A-C39 \\sim C38A-C38 \\sim C37A-C37
 with sigma of 0.02
 C32-C35 \\sim C32-C35A
 with sigma of 0.02
 C32-C33 \\sim C32-C33A
 with sigma of 0.02
 C32-C34 \\sim C32-C34A
 with sigma of 0.02
 C34A-C34 \\sim C33A-C33 \\sim C35A-C35
 with sigma of 0.02
 C34-C32 \\sim C34A-C32 \\sim C33A-C32 \\sim C33-C32 \\sim C35A-C32 \\sim
C35-C32
 with sigma of 0.005
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 C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A
\\sim C6A \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A:
within 2A with sigma of 0.02 and sigma for terminal atoms of 0.01 within 2A
C37 \\sim C38 \\sim C39 \\sim C37A \\sim C38A \\sim C39A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
C34 \\sim C34A \\sim C33A \\sim C33 \\sim C35A \\sim C35: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C33(0.8) H33A(0.8) H33B(0.8) H33C(0.8) C34(0.8) H34A(0.8)
 H34B(0.8) H34C(0.8) C35(0.8) H35A(0.8) H35B(0.8) H35C(0.8) C1(0.55) C2(0.55)
 C3(0.55) H3(0.55) C4(0.55) H4(0.55) C5(0.55) H5(0.55) C6(0.55) C7(0.55)
 H7(0.55) C8(0.55) H8A(0.55) H8B(0.55) H8C(0.55) C9(0.55) H9A(0.55) H9B(0.55)
 H9C(0.55) C10(0.55) H10(0.55) C11(0.55) H11A(0.55) H11B(0.55) H11C(0.55)
 C12(0.55) H12A(0.55) H12B(0.55) H12C(0.55) C37(0.8) H37A(0.8) H37B(0.8)
 H37C(0.8) C38(0.8) H38A(0.8) H38B(0.8) H38C(0.8) C39(0.8) H39A(0.8) H39B(0.8)
 H39C(0.8) C1A(0.45) C2A(0.45) C3A(0.45) H3A(0.45) C4A(0.45) H4A(0.45)
 C5A(0.45) H5A(0.45) C6A(0.45) C7A(0.45) H7A(0.45) C8A(0.45) H8AA(0.45)
 H8AB(0.45) H8AC(0.45) C9A(0.45) H9AA(0.45) H9AB(0.45) H9AC(0.45) C10A(0.45)
 H10A(0.45) C11A(0.45) H11D(0.45) H11E(0.45) H11F(0.45) C12A(0.45) H12D(0.45)
 H12E(0.45) H12F(0.45) C37A(0.2) H37D(0.2) H37E(0.2) H37F(0.2) C38A(0.2)
 H38D(0.2) H38E(0.2) H38F(0.2) C39A(0.2) H39D(0.2) H39E(0.2) H39F(0.2)
 C34A(0.2) H34D(0.2) H34E(0.2) H34F(0.2) C33A(0.2) H33D(0.2) H33E(0.2)
 H33F(0.2) C35A(0.2) H35D(0.2) H35E(0.2) H35F(0.2)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C28(H28), C31(H31), C46(H46), C49(H49), C64(H64), C67(H67),
 C70(H70), C7(H7), C10(H10), C7A(H7A), C10A(H10A)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C30(H30A,H30B), C54(H54A,H54B), C55(H55A,
 H55B), C69(H69A,H69B)
5.c Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C42(H42), C43(H43), C44(H44), C60(H60),
 C61(H61), C62(H62), C3(H3), C4(H4), C5(H5), C3A(H3A), C4A(H4A), C5A(H5A)
5.d Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C1A(C2A,C3A,C4A,C5A,C6A)
5.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C65(H65A,
 H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C72(H72A,H72B,H72C),
 C73(H73A,H73B,H73C), C74(H74A,H74B,H74C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC), C11A(H11D,H11E,H11F),
 C12A(H12D,H12E,H12F), C37A(H37D,H37E,H37F), C38A(H38D,H38E,H38F), C39A(H39D,
 H39E,H39F), C34A(H34D,H34E,H34F), C33A(H33D,H33E,H33F), C35A(H35D,H35E,H35F)
;
_shelx_res_checksum              51617
_shelx_hkl_checksum              1497
_olex2_submission_special_instructions 'No special instructions were received'