Rubidium and caesium aluminyls: synthesis, structures and reactivity in C–H bond activation of benzene
Gentner, Thomas X.; Evans, Matthew J.; Kennedy, Alan R.; Neale, Sam E.; McMullin, Claire L.; Coles, Martyn P.; Mulvey, Robert E.; Chemical Communications  (2022) –; doi:10.1039/D1CC05379E

data_7129516
_publ_section_title
;
 Rubidium and caesium aluminyls: synthesis, structures and reactivity in
 C--H bond activation of benzene
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05379E
_journal_year                    2022
_chemical_formula_sum            'C59 H99 Al2 Cs2 N4 O2 Si4'
_chemical_formula_weight         1328.56
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-08-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-21 deposited with the CCDC.	2021-12-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.7249(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.57265(17)
_cell_length_b                   17.60387(9)
_cell_length_c                   36.1042(2)
_cell_measurement_reflns_used    63680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.515
_cell_measurement_theta_min      2.562
_cell_volume                     14189.16(16)
_computing_cell_refinement       CrysalisPro
_computing_data_collection       CrysalisPro
_computing_data_reduction        CrysalisPro
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaky Synergy-i'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1063
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            106812
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         72.685
_diffrn_reflns_theta_min         2.584
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    9.189
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.13850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             5512
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.089
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         14056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0581
_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^)+(0.1236P)^2^+22.0259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1619
_refine_ls_wR_factor_ref         0.1633
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13626
_reflns_number_total             14056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05379e2.cif
_cod_data_source_block           alcs(non)_auto
_cod_original_cell_volume        14189.15(17)
_cod_database_code               7129516
_shelx_shelxl_version_number     2014/7
_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:
 C7(H7), C10(H10), C21(H21), C24(H24), C35(H35), C38(H38), C49(H49), C54(H54)
2.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C17(H17), C18(H18), C19(H19), C31(H31), C32(H32),
 C33(H33), C45(H45), C46(H46), C47(H47)
2.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,
 H58B,H58C), C59(H59A,H59B,H59C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              58410
_shelx_hkl_checksum              69357
_olex2_submission_special_instructions 'No special instructions were received'