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_7130184
_publ_section_title
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 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         'C64 H86 Al K N2 O4 Si2'
_chemical_formula_sum            'C64 H86 Al K N2 O4 Si2'
_chemical_formula_weight         1069.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-04-23 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.877(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7511(4)
_cell_length_b                   13.3392(2)
_cell_length_c                   20.8348(3)
_cell_measurement_reflns_used    10205
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.0030
_cell_measurement_theta_min      4.3270
_cell_volume                     5915.64(17)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_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  0.0209
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15239
_diffrn_reflns_point_group_measured_fraction_full 0.684
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.119
_diffrn_reflns_theta_min         3.911
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.686
_exptl_absorpt_correction_T_max  0.755
_exptl_absorpt_correction_T_min  0.426
_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            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.211
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 1942 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.027(7)
_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     683
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.365
_reflns_Friedel_fraction_full    0.371
_reflns_Friedel_fraction_max     0.364
_reflns_number_gt                7691
_reflns_number_total             7932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02333d2.cif
_cod_data_source_block           s20msh83-cpd11
_cod_database_code               7130184
_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.a Ternary CH refined with riding coordinates:
 C32(H32), C10(H10), C25(H25), C7(H7), C28(H28), C60(H60a)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C16(H16a,H16b), C58(H58a,H58b), C64(H64a,H64b), C59(H59a,
 H59b), C63(H63a,H63b), C57(H57a,H57b), C62(H62a,H62b), C61(H61a,H61b)
2.c Aromatic/amide H refined with riding coordinates:
 C40(H40), C39(H39), C37(H37), C36(H36), C4(H4), C42(H42), C5(H5), C38(H38),
 C3(H3), C44(H44), C45(H45), C56(H56), C23(H23), C43(H43), C55(H55), C49(H49),
 C53(H53), C54(H54), C52(H52), C50(H50), C47(H47), C22(H22), C21(H21), C46(H46),
  C48(H48)
2.d Idealised Me refined as rotating group:
 C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C11(H11a,H11b,H11c), C18(H18a,H18b,
 H18c), C13(H13a,H13b,H13c), C27(H27a,H27b,H27c), C9(H9c,H9a,H9b), C26(H26a,
 H26b,H26c), C8(H8a,H8b,H8c), C17(H17a,H17b,H17c), C30(H30a,H30b,H30c),
 C29(H29a,H29b,H29c)
;
_shelx_res_checksum              85553
_shelx_hkl_checksum              30159
_olex2_submission_special_instructions 'No special instructions were received'