On the Reactivity of Al-Group 11 (Cu, Ag, Au) Bonds
Hill, Michael; Liu, Han-Ying; Neale, Samuel E.; Mahon, Mary F.; McMullin, Claire Louise; Dalton Transactions  (2022) –; doi:10.1039/D2DT00404F

data_7709534
_publ_section_title
;
 On the Reactivity of Al-Group 11 (Cu, Ag, Au) Bonds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00404F
_journal_year                    2022
_chemical_formula_moiety         '2(C48 H84 Al Au N6 Si2)'
_chemical_formula_sum            'C106.5 H189 Al2 Au2 N12 Si4'
_chemical_formula_weight         2197.94
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-07 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.92320(10)
_cell_length_b                   31.73350(10)
_cell_length_c                   26.07640(10)
_cell_measurement_reflns_used    62887
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7430
_cell_measurement_theta_min      4.0690
_cell_volume                     12346.59(10)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            172051
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.505
_diffrn_reflns_theta_min         3.660
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.245
_exptl_absorpt_correction_T_max  0.776
_exptl_absorpt_correction_T_min  0.509
_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    1.182
_exptl_crystal_description       block
_exptl_crystal_F_000             4608
_exptl_crystal_size_max          0.106
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.047
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.210
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1118
_refine_ls_number_reflns         24603
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+4.0693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21807
_reflns_number_total             24603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00404f2.cif
_cod_data_source_block           s21msh19-cpd20
_cod_original_formula_sum        'C106.50 H189 Al2 Au2 N12 Si4'
_cod_database_code               7709534
_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
 N3-C32A \\sim N3-C32
 with sigma of 0.005
 C33-C32 \\sim C33A-C32A \\sim C34-C32 \\sim C34A-C32A
 with sigma of 0.005
 C34A-C33A \\sim C33-C34
 with sigma of 0.01
3. Others
 Fixed Sof: C32(0.63) H32(0.63) C33(0.63) H33A(0.63) H33B(0.63) H33C(0.63)
 C34(0.63) H34A(0.63) H34B(0.63) H34C(0.63) C32A(0.37) H32A(0.37) C34A(0.37)
 H34D(0.37) H34E(0.37) H34F(0.37) C33A(0.37) H33D(0.37) H33E(0.37) H33F(0.37)
4.a Ternary CH refined with riding coordinates:
 C58(H58), C91(H91), C76(H76), C43(H43), C25(H25), C7(H7), C46(H46), C94(H94),
 C39(H39), C87(H87), C55(H55), C28(H28), C73(H73), C80(H80), C10(H10), C32(H32),
  C32A(H32A)
4.b Secondary CH2 refined with riding coordinates:
 C63(H63A,H63B), C64(H64A,H64B), C15(H15A,H15B), C16(H16A,H16B)
4.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C71(H71), C3(H3), C69(H69), C70(H70), C4(H4), C21(H21), C51(H51),
 C52(H52), C5(H5), C23(H23), C22(H22)
4.d Idealised Me refined as rotating group:
 C93(H93A,H93B,H93C), C61(H61A,H61B,H61C), C92(H92A,H92B,H92C), C59(H59A,H59B,
 H59C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C62(H62A,H62B,H62C), C14(H14A,
 H14B,H14C), C96(H96A,H96B,H96C), C44(H44A,H44B,H44C), C26(H26A,H26B,H26C),
 C17(H17A,H17B,H17C), C36(H36A,H36B,H36C), C48(H48A,H48B,H48C), C47(H47A,H47B,
 H47C), C45(H45A,H45B,H45C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C86(H86A,
 H86B,H86C), C60(H60A,H60B,H60C), C78(H78A,H78B,H78C), C18(H18A,H18B,H18C),
 C38(H38A,H38B,H38C), C8(H8A,H8B,H8C), C77(H77A,H77B,H77C), C40(H40A,H40B,H40C),
  C74(H74A,H74B,H74C), C82(H82A,H82B,H82C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C88(H88A,H88B,H88C), C27(H27A,H27B,H27C), C57(H57A,H57B,H57C), C56(H56A,
 H56B,H56C), C81(H81A,H81B,H81C), C11(H11A,H11B,H11C), C33(H33A,H33B,H33C),
 C95(H95A,H95B,H95C), C41(H41A,H41B,H41C), C84(H84A,H84B,H84C), C75(H75A,H75B,
 H75C), C12(H12A,H12B,H12C), C89(H89A,H89B,H89C), C34(H34A,H34B,H34C),
 C34A(H34D,H34E,H34F), C33A(H33D,H33E,H33F)
;