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_1568434
_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(C74 H96 Al Cu2 N3 Si2), 2(C6 H14)'
_chemical_formula_sum            'C160 H220 Al2 Cu4 N6 Si4'
_chemical_formula_weight         2647.89
_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             2022-05-20
_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                97.9780(10)
_cell_angle_beta                 98.3410(10)
_cell_angle_gamma                96.908(2)
_cell_formula_units_Z            2
_cell_length_a                   13.2732(2)
_cell_length_b                   17.1411(3)
_cell_length_c                   34.2337(6)
_cell_measurement_reflns_used    35472
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      30.2900
_cell_measurement_theta_min      3.0130
_cell_volume                     7553.0(2)
_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 16.1468
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            128297
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.129
_diffrn_reflns_theta_min         3.000
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.649
_exptl_absorpt_correction_T_max  0.364
_exptl_absorpt_correction_T_min  0.145
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.164
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.604
_exptl_crystal_size_mid          0.472
_exptl_crystal_size_min          0.279
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1741
_refine_ls_number_reflns         38945
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+3.7224P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.1016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30685
_reflns_number_total             38945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00240c2.cif
_cod_data_source_block           e21msh09
_cod_depositor_comments
'Adding full bibliography for 1568428--1568438.cif.'
_cod_database_code               1568434
_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
 C4SA-C3SA = C4SA-C5SA = C6SA-C5SA = C2SA-C3SA
 1.54 with sigma of 0.005
 C6S-C5S = C5S-C4S = C4S-C3S = C3S-C2S = C2S-C1S
 1.54 with sigma of 0.005
 C2TA-C1TA = C3TA-C2TA = C5TA-C6TA = C5TA-C4TA = C3TA-C4TA
 1.54 with sigma of 0.005
 C2TA-C1TA = C3TA-C2TA = C3TA-C4TA = C5TA-C4TA = C5TA-C6TA
 1.54 with sigma of 0.005
 C1TA-C3TA = C2TA-C4TA
 2.555 with sigma of 0.01
 C3TA-C5TA = C6TA-C4TA
 2.555 with sigma of 0.01
 C6SA-C4SA \\sim C5SA-C3SA
 with sigma of 0.005
 C3S-C1S \\sim C1SA-C3SA \\sim C2SA-C4SA
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C1SA \\sim C2SA \\sim C3SA \\sim C4SA \\sim C5SA \\sim C6SA \\sim C1S \\sim C2S
\\sim C3S \\sim C4S \\sim C5S \\sim C6S: within 2A with sigma of 0.015 and
sigma for terminal atoms of 0.01 within 2A
C1T \\sim C2T \\sim C3T \\sim C4T \\sim C5T \\sim C6T \\sim C1TA \\sim C2TA
\\sim C3TA \\sim C4TA \\sim C5TA \\sim C6TA: within 2A with sigma of 0.015 and
sigma for terminal atoms of 0.01 within 2A
4. Others
 Fixed Sof: C1T(0.75) H1TA(0.75) H1TB(0.75) H1TC(0.75) C2T(0.75) H2TA(0.75)
 H2TB(0.75) C3T(0.75) H3TA(0.75) H3TB(0.75) C4T(0.75) H4TA(0.75) H4TB(0.75)
 C5T(0.75) H5TA(0.75) H5TB(0.75) C6T(0.75) H6TA(0.75) H6TB(0.75) H6TC(0.75)
 C1TA(0.25) H1TD(0.25) H1TE(0.25) H1TF(0.25) C2TA(0.25) H2TC(0.25) H2TD(0.25)
 C3TA(0.25) H3TC(0.25) H3TD(0.25) C4TA(0.25) H4TC(0.25) H4TD(0.25) C5TA(0.25)
 H5TC(0.25) H5TD(0.25) C6TA(0.25) H6TD(0.25) H6TE(0.25) H6TF(0.25) C1SA(0.45)
 H1SA(0.45) H1SB(0.45) H1SC(0.45) C2SA(0.45) H2SA(0.45) H2SB(0.45) C3SA(0.45)
 H3SA(0.45) H3SB(0.45) C4SA(0.45) H4SA(0.45) H4SB(0.45) C5SA(0.45) H5SA(0.45)
 H5SB(0.45) C6SA(0.45) H6SA(0.45) H6SC(0.45) H6SB(0.45) C1S(0.55) H1SD(0.55)
 H1SE(0.55) H1SF(0.55) C2S(0.55) H2SD(0.55) H2SC(0.55) C3S(0.55) H3SC(0.55)
 H3SD(0.55) C4S(0.55) H4SC(0.55) H4SD(0.55) C5S(0.55) H5SC(0.55) H5SD(0.55)
 C6S(0.55) H6SD(0.55) H6SE(0.55) H6SF(0.55)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C25(H25), C28(H28), C45(H45), C48(H48), C81(H81), C84(H84),
 C99(H99), C102(H102), C119(H119), C122(H122)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C35(H35A,H35B), C89(H89A,H89B), C90(H90A,
 H90B), C109(H10S,H10T), C2T(H2TA,H2TB), C3T(H3TA,H3TB), C4T(H4TA,H4TB),
 C5T(H5TA,H5TB), C2TA(H2TC,H2TD), C3TA(H3TC,H3TD), C4TA(H4TC,H4TD), C5TA(H5TC,
 H5TD), C2SA(H2SA,H2SB), C3SA(H3SA,H3SB), C4SA(H4SA,H4SB), C5SA(H5SA,H5SB),
 C2S(H2SD,H2SC), C3S(H3SC,H3SD), C4S(H4SC,H4SD), C5S(H5SC,H5SD)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C21(H21), C22(H22), C23(H23), C41(H41), C42(H42),
 C43(H43), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68), C70(H70), C71(H71), C72(H72), C73(H73),
 C74(H74), C77(H77), C78(H78), C79(H79), C95(H95), C96(H96), C97(H97),
 C115(H115), C116(H116), C117(H117), C128(H128), C129(H129), C130(H130),
 C131(H131), C132(H132), C138(H138), C139(H139), C140(H140), C141(H141),
 C142(H142), C144(H144), C145(H145), C146(H146), C147(H147), C148(H148)
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), C37(H37A,H37B,H37C),
 C38(H38A,H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C50(H50A,H50B,H50C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C85(H85A,
 H85B,H85C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C),
 C91(H91A,H91B,H91C), C92(H92A,H92B,H92C), C100(H10A,H10B,H10C), C101(H10D,H10E,
 H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C107(H10M,H10N,H10O),
 C108(H10P,H10Q,H10R), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C120(H12D,
 H12E,H12F), C121(H12G,H12H,H12I), C123(H12J,H12K,H12L), C124(H12M,H12N,H12O),
 C1T(H1TA,H1TB,H1TC), C6T(H6TA,H6TB,H6TC), C1TA(H1TD,H1TE,H1TF), C6TA(H6TD,H6TE,
 H6TF), C1SA(H1SA,H1SB,H1SC), C6SA(H6SA,H6SC,H6SB), C1S(H1SD,H1SE,H1SF),
 C6S(H6SD,H6SE,H6SF)
;
_shelx_res_checksum              52952
_shelx_hkl_checksum              90832