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_7709533
_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 Ag Al N6 Si2)'
_chemical_formula_sum            'C96 H168 Ag2 Al2 N12 Si4'
_chemical_formula_weight         1872.47
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-25
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3646(2)
_cell_length_b                   10.92730(10)
_cell_length_c                   39.1524(3)
_cell_measurement_reflns_used    59502
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.8170
_cell_measurement_theta_min      4.1860
_cell_volume                     10423.91(15)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0734
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_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           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            121205
_diffrn_reflns_point_group_measured_fraction_full 0.743
_diffrn_reflns_point_group_measured_fraction_max 0.740
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.374
_diffrn_reflns_theta_min         3.800
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.973
_exptl_absorpt_correction_T_max  0.358
_exptl_absorpt_correction_T_min  0.023
_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    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.054
_refine_diff_density_max         2.822
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.035(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         15006
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0571
_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^)+(0.1145P)^2^+0.5429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.459
_reflns_Friedel_fraction_full    0.480
_reflns_Friedel_fraction_max     0.473
_reflns_number_gt                14174
_reflns_number_total             15006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00404f2.cif
_cod_data_source_block           s21msh3-cpd19
_cod_database_code               7709533
_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
 C85-C83 \\sim C85A-C83A \\sim C37A-C35A \\sim C37-C35
 with sigma of 0.005
 C38A-C37A \\sim C38-C37 \\sim C36A-C35A \\sim C36-C35 \\sim C86A-C85A \\sim
C86-C85 \\sim C84A-C83A 
 C84-C83
 with sigma of 0.005
 N3-C31 \\sim N3A-C31 \\sim N4A-C31 \\sim N4-C31 \\sim N10A-C79 \\sim N10-C79
\\sim N9-C79 \\sim N9A-C79
 with sigma of 0.005
 N10-C85 \\sim N10A-C85A \\sim N9A-C83A \\sim N9-C83 \\sim N3-C35 \\sim
N3A-C35A \\sim N4-C37 \\sim N4A-C37A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
N4 \\sim N4A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
N3 \\sim N3A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
N10 \\sim N10A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.01
N9 \\sim N9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: N3(0.55) N4(0.55) N3A(0.45) N4A(0.45) H32(0.55) H32A(0.45)
 H39(0.55) H39A(0.45) C35(0.55) C36(0.55) H36A(0.55) H36B(0.55) H36C(0.55)
 C37(0.55) C38(0.55) H38A(0.55) H38B(0.55) H38C(0.55) C35A(0.45) C36A(0.45)
 H36D(0.45) H36E(0.45) H36F(0.45) C37A(0.45) C38A(0.45) H38D(0.45) H38E(0.45)
 H38F(0.45) N9(0.55) N10(0.55) N9A(0.45) N10A(0.45) H80(0.55) H80A(0.45)
 H87(0.55) H87A(0.45) C83(0.55) C84(0.55) H84A(0.55) H84B(0.55) H84C(0.55)
 C85(0.55) C86(0.55) H86A(0.55) H86B(0.55) H86C(0.55) C83A(0.45) C84A(0.45)
 H84D(0.45) H84E(0.45) H84F(0.45) C85A(0.45) C86A(0.45) H86D(0.45) H86E(0.45)
 H86F(0.45)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C25(H25), C28(H28), C32(H32), C32(H32A), C39(H39),
 C39(H39A), C43(H43), C46(H46), C55(H55), C58(H58), C73(H73), C76(H76),
 C80(H80), C80(H80A), C87(H87), C87(H87A), C91(H91), C94(H94)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C63(H63A,H63B), C64(H64A,H64B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C21(H21), C22(H22), C23(H23), C51(H51), C52(H52),
 C53(H53), C69(H69), C70(H70), C71(H71)
5.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), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C),
 C36A(H36D,H36E,H36F), C38A(H38D,H38E,H38F), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C74(H74A,H74B,H74C),
 C75(H75A,H75B,H75C), C77(H77A,H77B,H77C), C78(H78A,H78B,H78C), C81(H81A,H81B,
 H81C), C82(H82A,H82B,H82C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C92(H92A,
 H92B,H92C), C93(H93A,H93B,H93C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C),
 C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C84A(H84D,H84E,H84F), C86A(H86D,H86E,
 H86F)
;