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_7709530
_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         'C42 H77 Al Cu N2 P Si2'
_chemical_formula_sum            'C42 H77 Al Cu N2 P Si2'
_chemical_formula_weight         787.72
_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             2021-09-06
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2022-01-07 deposited with the CCDC.	2022-02-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.2510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.45810(10)
_cell_length_b                   16.19060(10)
_cell_length_c                   23.05460(10)
_cell_measurement_reflns_used    34874
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.8510
_cell_measurement_theta_min      4.4880
_cell_volume                     4622.56(5)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -102.00 -24.00   1.00    1.00    --  -37.15 -57.00 -90.00   78
  2  \w    -63.00  31.00   1.00    1.00    --  -37.15  19.00  90.00   94
  3  \w    -60.00  31.00   1.00    1.00    --  -37.15  19.00-180.00   91
  4  \w     23.00  98.00   1.00    1.00    --   37.15  57.00-150.00   75
  5  \w      6.00  68.00   1.00    1.00    --   37.15 -99.00  30.00   62
  6  \w     39.00  79.00   1.00    1.00    --   37.15-125.00 150.00   40
  7  \w     36.00  89.00   1.00    1.00    --   37.15-125.00 -90.00   53
  8  \w     82.00 108.00   1.00    2.50    --  109.00-111.00  30.00   26
  9  \w     96.00 131.00   1.00    2.50    --  109.00  30.00  30.00   35
 10  \w     51.00  95.00   1.00    2.50    --  109.00 -52.00  54.74   44
 11  \w     96.00 122.00   1.00    2.50    --  109.00 -30.00 120.00   26
 12  \w     41.00  90.00   1.00    2.50    --  109.00 -94.00  30.00   49
 13  \w    150.00 175.00   1.00    2.50    --  109.00  77.00  60.00   25
 14  \w     46.00  72.00   1.00    2.50    --  109.00 -77.00 -90.00   26
 15  \w     41.00  73.00   1.00    2.50    --  109.00 -30.00 120.00   32
 16  \w    106.00 176.00   1.00    2.50    --  109.00  15.00 150.00   70
 17  \w     42.00  68.00   1.00    2.50    --  109.00 -45.00-150.00   26
 18  \w     82.00 108.00   1.00    2.50    --  109.00-111.00 -90.00   26
 19  \w     47.00 122.00   1.00    2.50    --  109.00 -30.00-150.00   75
 20  \w     79.00 108.00   1.00    2.50    --  109.00-111.00-180.00   29
 21  \w     95.00 164.00   1.00    2.50    --  109.00  30.00  60.00   69
 22  \w     51.00  98.00   1.00    2.50    --  109.00 -94.00 -90.00   47
 23  \w     81.00 122.00   1.00    2.50    --  109.00  15.00   0.00   41
 24  \w     40.00 104.00   1.00    2.50    --  109.00-111.00 150.00   64
 25  \w     49.00  74.00   1.00    2.50    --  109.00-111.00  60.00   25
 26  \w     77.00 125.00   1.00    2.50    --  109.00 -45.00  90.00   48
 27  \w     47.00  91.00   1.00    2.50    --  109.00 -61.00 -60.00   44
 28  \w     98.00 124.00   1.00    2.50    --  109.00  30.00  90.00   26
 29  \w     63.00 140.00   1.00    2.50    --  109.00 -15.00  60.00   77
 30  \w     51.00 106.00   1.00    2.50    --  109.00-111.00-150.00   55
 31  \w    147.00 173.00   1.00    2.50    --  109.00  77.00 120.00   26
 32  \w     75.00 102.00   1.00    2.50    --  109.00-111.00-120.00   27
 33  \w     60.00 106.00   1.00    2.50    --  109.00-111.00  90.00   46
 34  \w     65.00  91.00   1.00    2.50    --  109.00 -94.00  60.00   26
 35  \w     93.00 162.00   1.00    2.50    --  109.00  45.00 -90.00   69
 36  \w     41.00  66.00   1.00    2.50    --  109.00-111.00 -90.00   25
 37  \w     43.00  94.00   1.00    2.50    --  109.00 -77.00-150.00   51
 38  \w     41.00 107.00   1.00    2.50    --  109.00-111.00 -30.00   66
 39  \w    106.00 159.00   1.00    2.50    --  109.00  15.00  30.00   53
 40  \w     93.00 130.00   1.00    2.50    --  109.00 -77.00 -90.00   37
 41  \w     78.00 119.00   1.00    2.50    --  109.00 -61.00  60.00   41
 42  \w    111.00 150.00   1.00    2.50    --  109.00  45.00-150.00   39
 43  \w     41.00  74.00   1.00    2.50    --  109.00 -30.00  30.00   33
 44  \w     90.00 126.00   1.00    2.50    --  109.00 -30.00  30.00   36
 45  \w     71.00 108.00   1.00    2.50    --  109.00-111.00 120.00   37
 46  \w     97.00 139.00   1.00    2.50    --  109.00  45.00-120.00   42
 47  \w     61.00  91.00   1.00    2.50    --  109.00 -77.00-180.00   30
 48  \w     65.00  91.00   1.00    2.50    --  109.00 -77.00   0.00   26
 49  \w     44.00  78.00   1.00    2.50    --  109.00 -77.00  60.00   34
 50  \w     85.00 110.00   1.00    2.50    --  109.00 -77.00  60.00   25
 51  \w    100.00 126.00   1.00    2.50    --  109.00 -81.00  79.77   26
 52  \w    106.00 149.00   1.00    2.50    --  109.00 111.00-150.00   43
 53  \w     67.00  93.00   1.00    2.50    --  109.00 -61.00 -90.00   26
 54  \w     72.00  97.00   1.00    2.50    --  109.00 178.00  30.00   25
 55  \w     93.00 118.00   1.00    2.50    --  109.00 -30.00   0.00   25
 56  \w     93.00 118.00   1.00    2.50    --  109.00  15.00-180.00   25
 57  \w     53.00  87.00   1.00    2.50    --  109.00 -40.00 -12.38   34
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0179060000
_diffrn_orient_matrix_UB_12      0.0037839000
_diffrn_orient_matrix_UB_13      0.0650164000
_diffrn_orient_matrix_UB_21      0.0165932000
_diffrn_orient_matrix_UB_22      0.0942922000
_diffrn_orient_matrix_UB_23      -0.0003723000
_diffrn_orient_matrix_UB_31      -0.1219700000
_diffrn_orient_matrix_UB_32      0.0122559000
_diffrn_orient_matrix_UB_33      -0.0170775000
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            58916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.795
_diffrn_reflns_theta_min         3.858
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.876
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.209
_exptl_crystal_size_mid          0.191
_exptl_crystal_size_min          0.158
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         9197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0365P)^2^+1.7360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0724
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8728
_reflns_number_total             9197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00404f2.cif
_cod_data_source_block           s21msh21_1_cpd23
_cod_database_code               7709530
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N Al Cu P'
_reflns_odcompleteness_completeness 97.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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), C28(H28), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15a,H15b), C16(H16a,H16b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C23(H23), C22(H22), C21(H21)
2.d Idealised Me refined as rotating group:
 C36(H36a,H36b,H36c), C32(H32a,H32b,H32c), C38(H38a,H38b,H38c), C14(H14a,H14b,
 H14c), C18(H18a,H18b,H18c), C41(H41a,H41b,H41c), C40(H40a,H40b,H40c), C42(H42a,
 H42b,H42c), C17(H17a,H17b,H17c), C34(H34a,H34b,H34c), C33(H33a,H33b,H33c),
 C37(H37a,H37b,H37c), C12(H12a,H12b,H12c), C26(H26a,H26b,H26c), C13(H13a,H13b,
 H13c), C9(H9a,H9b,H9c), C8(H8a,H8b,H8c), C29(H29a,H29b,H29c), C27(H27a,H27b,
 H27c), C11(H11a,H11b,H11c), C30(H30a,H30b,H30c)
;
_shelx_res_checksum              25687