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_7130183
_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         'C37 H64 Al K N2 O Si2, 0.5(C6 H6)'
_chemical_formula_sum            'C40 H67 Al K N2 O Si2'
_chemical_formula_weight         714.21
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2022-04-19 deposited with the CCDC.	2022-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.35550(10)
_cell_length_b                   23.00870(10)
_cell_length_c                   18.34080(10)
_cell_measurement_reflns_used    44961
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.9000
_cell_measurement_theta_min      4.5330
_cell_volume                     8589.98(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            112622
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.967
_diffrn_reflns_theta_min         3.770
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.035
_exptl_absorpt_correction_T_max  0.556
_exptl_absorpt_correction_T_min  0.112
_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    1.105
_exptl_crystal_description       block
_exptl_crystal_F_000             3112
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.973
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         8574
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0762P)^2^+3.4785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7920
_reflns_number_total             8574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc02333d2.cif
_cod_data_source_block           s21msh66-cpd13
_cod_database_code               7130183
_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
 C14-H27 \\sim C14-H30 \\sim C14-H29 \\sim C11-H50
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C38A \\sim C38 \\sim C39 \\sim C40 \\sim C39A \\sim C40A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C38(0.5) H35(0.5) C39(0.5) H8(0.5) C40(0.5) H11(0.5) C40A(0.5)
 H13(0.5) C39A(0.5) H15(0.5) C38A(0.5) H17(0.5)
5.a Ternary CH refined with riding coordinates:
 C28(H37), C10(H43), C25(H9), C7(H7), C35(H6)
5.b Secondary CH2 refined with riding coordinates:
 C15(H63,H57), C16(H64,H49)
5.c Aromatic/amide H refined with riding coordinates:
 C5(H21), C23(H41), C4(H34), C3(H59), C21(H20), C22(H48), C38(H35), C39(H8),
 C40(H11), C40A(H13), C39A(H15), C38A(H17)
5.d Fitted hexagon refined as free rotating group:
 C38(C39,C40,C40A,C39A,C38A)
5.e Idealised Me refined as rotating group:
 C17(H4,H16,H10), C18(H33,H47,H62), C13(H45,H56,H58), C26(H67,H68,H70),
 C27(H19,H28,H24), C12(H2,H36,H22), C30(H25,H53,H18), C29(H51,H12,H42), C34(H5,
 H23,H61), C11(H54,H44,H50), C9(H3,H40,H32), C36(H52,H39,H55), C33(H65,H31,H66),
  C8(H14,H69,H60), C37(H71,H46,H26)
;
_shelx_res_checksum              30223
_shelx_hkl_checksum              65075
_olex2_submission_special_instructions 'No special instructions were received'