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_7709532
_publ_section_title
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 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         'C49 H91 Al Cu N4 P Si2'
_chemical_formula_sum            'C49 H91 Al Cu N4 P Si2'
_chemical_formula_weight         913.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-09
_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                 106.3000(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.4042(2)
_cell_length_b                   12.84890(10)
_cell_length_c                   21.4769(2)
_cell_measurement_reflns_used    34370
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7900
_cell_measurement_theta_min      4.0380
_cell_volume                     5404.31(9)
_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 1.000
_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  0.0485
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            71855
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.124
_diffrn_reflns_theta_min         3.522
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.678
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.342
_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    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.358
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.253
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     665
_refine_ls_number_reflns         10645
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0652P)^2^+1.8526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9875
_reflns_number_total             10645
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00404f2.cif
_cod_data_source_block           s21msh11-cpd24
_cod_database_code               7709532
_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
 P1-C35 \\sim P1-C35A
 with sigma of 0.02
 C35-C36 \\sim C35A-C36A
 with sigma of 0.02
 C35-C37 \\sim C35A-C37A
 with sigma of 0.02
 C35-C38 \\sim C35A-C38A
 with sigma of 0.02
 P1-C36 \\sim P1-C36A
 with sigma of 0.04
 P1-C37 \\sim P1-C37A
 with sigma of 0.04
 P1-C38 \\sim P1-C38A
 with sigma of 0.04
 C36-C37 \\sim C36A-C37A
 with sigma of 0.04
 C36-C38 \\sim C36A-C38A
 with sigma of 0.04
 C37-C38 \\sim C37A-C38A
 with sigma of 0.04
 P1-C31 \\sim P1-C31A
 with sigma of 0.02
 C31-C32 \\sim C31A-C32A
 with sigma of 0.02
 C31-C33 \\sim C31A-C33A
 with sigma of 0.02
 C31-C34 \\sim C31A-C34A
 with sigma of 0.02
 P1-C32 \\sim P1-C32A
 with sigma of 0.04
 P1-C33 \\sim P1-C33A
 with sigma of 0.04
 P1-C34 \\sim P1-C34A
 with sigma of 0.04
 C32-C33 \\sim C32A-C33A
 with sigma of 0.04
 C32-C34 \\sim C32A-C34A
 with sigma of 0.04
 C33-C34 \\sim C33A-C34A
 with sigma of 0.04
 P1-C39 \\sim P1-C39A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C39-C41 \\sim C39A-C41A
 with sigma of 0.02
 C39-C42 \\sim C39A-C42A
 with sigma of 0.02
 P1-C40 \\sim P1-C40A
 with sigma of 0.04
 P1-C41 \\sim P1-C41A
 with sigma of 0.04
 P1-C42 \\sim P1-C42A
 with sigma of 0.04
 C40-C41 \\sim C40A-C41A
 with sigma of 0.04
 C40-C42 \\sim C40A-C42A
 with sigma of 0.04
 C41-C42 \\sim C41A-C42A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C36 \\sim C37 \\sim C38 \\sim C36A \\sim C37A \\sim C38A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
C32 \\sim C33 \\sim C34 \\sim C32A \\sim C33A \\sim C34A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
C40 \\sim C41 \\sim C42 \\sim C40A \\sim C41A \\sim C42A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01
C39 \\sim C39A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01
C35 \\sim C35A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01
C31 \\sim C31A: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.01
4. Others
 Fixed Sof: C31(0.65) C32(0.65) H32A(0.65) H32B(0.65) H32C(0.65) C33(0.65)
 H33A(0.65) H33B(0.65) H33C(0.65) C34(0.65) H34A(0.65) H34B(0.65) H34C(0.65)
 C35(0.65) C36(0.65) H36A(0.65) H36B(0.65) H36C(0.65) C37(0.65) H37A(0.65)
 H37B(0.65) H37C(0.65) C38(0.65) H38A(0.65) H38B(0.65) H38C(0.65) C39(0.65)
 C40(0.65) H40A(0.65) H40B(0.65) H40C(0.65) C41(0.65) H41A(0.65) H41B(0.65)
 H41C(0.65) C42(0.65) H42A(0.65) H42B(0.65) H42C(0.65) C31A(0.35) C32A(0.35)
 H32D(0.35) H32E(0.35) H32F(0.35) C33A(0.35) H33D(0.35) H33E(0.35) H33F(0.35)
 C34A(0.35) H34D(0.35) H34E(0.35) H34F(0.35) C35A(0.35) C36A(0.35) H36D(0.35)
 H36E(0.35) H36F(0.35) C37A(0.35) H37D(0.35) H37E(0.35) H37F(0.35) C38A(0.35)
 H38D(0.35) H38E(0.35) H38F(0.35) C39A(0.35) C40A(0.35) H40D(0.35) H40E(0.35)
 H40F(0.35) C41A(0.35) H41D(0.35) H41E(0.35) H41F(0.35) C42A(0.35) H42D(0.35)
 H42E(0.35) H42F(0.35)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C25(H25), C28(H28), C44(H44), C47(H47)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C21(H21), C22(H22), C23(H23)
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), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C),
 C49(H49A,H49B,H49C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,
 H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C32A(H32D,H32E,H32F),
 C33A(H33D,H33E,H33F), C34A(H34D,H34E,H34F), C36A(H36D,H36E,H36F), C37A(H37D,
 H37E,H37F), C38A(H38D,H38E,H38F), C40A(H40D,H40E,H40F), C41A(H41D,H41E,H41F),
 C42A(H42D,H42E,H42F)
;