Direct observation of β-alkynyl eliminations from unstrained propargylic alkoxide Cu(i) complexes by C-C bond cleavage.
Tran, Ba L.; Fuller, 3rd, Jack T; Erickson, Jeremy D.; Ginovska, Bojana; Raugei, Simone; Chemical science 15 (2024) 17481–17489; doi:10.1039/d4sc02982h

data_1572667
_publ_section_title
;
 Direct observation of &#x3b2;-alkynyl eliminations from unstrained
 propargylic alkoxide Cu(i) complexes by C-C bond cleavage.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              17481
_journal_page_last               17489
_journal_paper_doi               10.1039/d4sc02982h
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C84 H66 Cu2 Fe2 P4'
_chemical_formula_sum            'C84 H66 Cu2 Fe2 P4'
_chemical_formula_weight         1438.02
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-03-25
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-04 deposited with the CCDC.	2024-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   21.9730(3)
_cell_length_b                   19.4588(4)
_cell_length_c                   45.8368(9)
_cell_measurement_reflns_used    9432
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.502
_cell_measurement_theta_min      2.332
_cell_volume                     19598.4(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            296050
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         2.004
_exptl_absorpt_coefficient_mu    1.224
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0571 before and 0.0473 after correction. The Ratio of minimum to maximum transmission is 0.9174. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             8880
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.206
_refine_diff_density_max         0.878
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1244
_refine_ls_number_reflns         22502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+49.8814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20639
_reflns_number_total             22502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc02982h3.cif
_cod_data_source_block           jdebt134
_cod_depositor_comments
'Adding full bibliography for 1572662--1572672.cif.'
_cod_database_code               1572667
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.710
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C108(H108), C103(H103), C98(H98), C101(H101), C96(H96), C68(H68), C104(H104),
 C114(H114), C100(H100), C51(H51), C99(H99), C86(H86), C42(H42), C58(H58),
 C64(H64), C46(H46), C56(H56), C90(H90), C106(H106), C54(H54), C105(H105),
 C48(H48), C109(H109), C36(H36), C112(H112), C87(H87), C49(H49), C59(H59),
 C53(H53), C50(H50), C52(H52), C118(H118), C67(H67), C95(H95), C81(H81),
 C126(H126), C62(H62), C110(H110), C88(H88), C22(H22), C65(H65), C92(H92),
 C117(H117), C111(H111), C40(H40), C89(H89), C17(H17), C115(H115), C93(H93),
 C2(H2), C80(H80), C28(H28), C12(H12), C94(H94), C84(H84), C66(H66), C45(H45),
 C43(H43), C60(H60), C122(H122), C39(H39), C116(H116), C44(H44), C124(H124),
 C37(H37), C125(H125), C61(H61), C38(H38), C76(H76), C21(H21), C82(H82),
 C123(H123), C34(H34), C8(H8), C14(H14), C24(H24), C32(H32), C27(H27), C19(H19),
  C30(H30), C16(H16), C33(H33), C25(H25), C26(H26), C9(H9), C11(H11), C15(H15),
 C6(H6), C10(H10), C20(H20), C75(H75), C31(H31), C83(H83), C74(H74), C72(H72),
 C3(H3), C5(H5), C4(H4), C73(H73)
;
_olex2_submission_special_instructions 'No special instructions were received'