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_1568429
_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         'C53 H88 Al Cu N4 Si2'
_chemical_formula_sum            'C53 H88 Al Cu N4 Si2'
_chemical_formula_weight         927.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-26
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-01-04 deposited with the CCDC.	2023-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.41970(10)
_cell_length_b                   13.52450(10)
_cell_length_c                   19.68390(10)
_cell_measurement_reflns_used    33935
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.7130
_cell_measurement_theta_min      4.7700
_cell_volume                     5552.70(6)
_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 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0313
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49961
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.852
_diffrn_reflns_theta_min         3.895
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.379
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78945
_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    1.110
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.411
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 4209 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.000(6)
_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     601
_refine_ls_number_reflns         9866
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0450P)^2^+1.7668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0729
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    0.794
_reflns_Friedel_fraction_max     0.782
_reflns_number_gt                9739
_reflns_number_total             9866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc00240c2.cif
_cod_data_source_block           s21msh75
_cod_depositor_comments
'Adding full bibliography for 1568428--1568438.cif.'
_cod_original_cell_volume        5552.69(6)
_cod_database_code               1568429
_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
 C43-C46 \\sim C43-C46A
 with sigma of 0.02
 C49-C48 \\sim C49A-C48A
 with sigma of 0.005
 C48-C47 \\sim C48A-C47A
 with sigma of 0.005
 C46-C43 \\sim C46A-C43
 with sigma of 0.005
 C47A-C46A \\sim C47-C46
 with sigma of 0.005
 C47-C49 \\sim C47A-C49A
 with sigma of 0.005
 C46-C48 \\sim C46A-C48A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C47 \\sim C48 \\sim C49 \\sim C47A \\sim C48A \\sim C49A: within 2A with sigma
of 0.02 and sigma for terminal atoms of 0.01 within 2A
Uanis(C46A) = Uanis(C46)
4. Others
 Fixed Sof: C46(0.85) H46A(0.85) H46B(0.85) C47(0.85) H47A(0.85) H47B(0.85)
 C48(0.85) H48A(0.85) H48B(0.85) C49(0.85) H49A(0.85) H49B(0.85) H49C(0.85)
 C46A(0.15) H46C(0.15) H46D(0.15) C47A(0.15) H47C(0.15) H47D(0.15) C48A(0.15)
 H48C(0.15) H48D(0.15) C49A(0.15) H49D(0.15) H49E(0.15) H49F(0.15)
5.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C25(H25), C28(H28), C32(H32), C39(H39)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,
 H52B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C46A(H46C,H46D),
 C47A(H47C,H47D), C48A(H48C,H48D)
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), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C53(H53A,H53B,
 H53C), C49(H49A,H49B,H49C), C49A(H49D,H49E,H49F)
;
_shelx_res_checksum              14819
_shelx_hkl_checksum              61598