Structural snapshots of an Al-Cu bond-mediated transformation of terminal acetylenes.
Liu, Han-Ying; Neale, Samuel E.; Hill, Michael S.; Mahon, Mary F.; McMullin, Claire L.; Chemical science 14 (2023) 2866–2876; doi:10.1039/d3sc00240c

data_1568430
_publ_section_title
;
 Structural snapshots of an Al-Cu bond-mediated transformation of terminal
 acetylenes.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              2866
_journal_page_last               2876
_journal_paper_doi               10.1039/d3sc00240c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C20 H31 Cu0.5 N), C46 H60 Al N2 Si2'
_chemical_formula_sum            'C86 H122 Al Cu N4 Si2'
_chemical_formula_weight         1358.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-08-04
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-01-04 deposited with the CCDC.	2023-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                81.8850(10)
_cell_angle_beta                 86.3370(10)
_cell_angle_gamma                74.292(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2250(2)
_cell_length_b                   12.4368(2)
_cell_length_c                   27.9562(4)
_cell_measurement_reflns_used    28805
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7570
_cell_measurement_theta_min      4.2270
_cell_volume                     4049.28(12)
_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 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            56874
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.913
_diffrn_reflns_theta_min         3.723
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.093
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.674
_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    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.054
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     878
_refine_ls_number_reflns         16041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0495P)^2^+0.9458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0947
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14230
_reflns_number_total             16041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00240c2.cif
_cod_data_source_block           s21msh70
_cod_depositor_comments
'Adding full bibliography for 1568428--1568438.cif.'
_cod_database_code               1568430
_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.a Ternary CH refined with riding coordinates:
 C38(H38), C41(H41), C38A(H38A), C41A(H41A), C7(H7), C10(H10), C25(H25),
 C28(H28)
2.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C47A(H47C,H47D), C15(H15A,H15B), C16(H16A,H16B)
2.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C35(H35), C36(H36), C34A(H34A), C35A(H35A), C36A(H36A), C3(H3),
 C4(H4), C5(H5), C21(H21), C22(H22), C23(H23), C56(H56), C57(H57), C58(H58),
 C59(H59), C60(H60), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
2.d Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F), C42A(H42D,H42E,H42F),
 C43A(H43D,H43E,H43F), C45A(H45D,H45E,H45F), C46A(H46D,H46E,H46F), C49A(H49D,
 H49E,H49F), C50A(H50D,H50E,H50F), 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)
;
_shelx_res_checksum              96525
_shelx_hkl_checksum              2229