Stepwise alkyne insertion in Au(i) acetylides: influence of the nuclearity.
Cayuela-Castillo, Juan; Fernández-de-Córdova, Francisco J; See, Matthew S.; Fernández, Israel; Ríos, Pablo; Chemical science 16 (2025) 4684–4694; doi:10.1039/d4sc08227c

data_1573907
_publ_section_title
;
 Stepwise alkyne insertion in Au(i) acetylides: influence of the
 nuclearity.
;
_journal_issue                   11
_journal_name_full               'Chemical science'
_journal_page_first              4684
_journal_page_last               4694
_journal_paper_doi               10.1039/d4sc08227c
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         '2(C66 H80 Au2 N4 O2), 0.625[C6H6], 3[C6H6]'
_chemical_formula_sum            'C150 H178 Au4 N8 O4'
_chemical_formula_weight         2944.86
_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             2024-12-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-04 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                93.781(5)
_cell_angle_beta                 94.261(4)
_cell_angle_gamma                100.703(4)
_cell_formula_units_Z            4
_cell_length_a                   13.4415(13)
_cell_length_b                   29.354(3)
_cell_length_c                   36.128(4)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      2.236
_cell_volume                     13922(3)
_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  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 'Bruker Photon II area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0601
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50762
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.256
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1691 before and 0.1084 after correction.
The Ratio of minimum to maximum transmission is 0.7047.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       prism
_exptl_crystal_F_000             5928
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Benzene - Pentane'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.283
_refine_diff_density_min         -2.563
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3167
_refine_ls_number_reflns         50762
_refine_ls_number_restraints     3475
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0864
_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^)+(0.0329P)^2^+430.7385P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.1960
_reflns_Friedel_coverage         0.000
_reflns_number_gt                44158
_reflns_number_total             50762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc08227c6.cif
_cod_data_source_block           pr1924a
_cod_depositor_comments
'Adding full bibliography for 1573902--1573910.cif.'
_cod_original_cell_volume        13921(3)
_cod_database_code               1573907
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.225
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8144(7)
 0.1856(7)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C47-C48 = C44-C45 = C45-C46
 1.37 with sigma of 0.02
 C295-C296 = C298-C299 = C299-C300
 1.37 with sigma of 0.02
 C301-C302 = C304-C305 = C305-C306
 1.37 with sigma of 0.02
 C47-C46
 1.38 with sigma of 0.02
 C295-C300
 1.38 with sigma of 0.02
 C48-C43 = C43-C44
 1.36 with sigma of 0.02
 C301-C306
 1.38 with sigma of 0.02
 C302-C303 = C303-C304
 1.36 with sigma of 0.02
 C296-C297 = C297-C298
 1.36 with sigma of 0.02
 C283-C284 = C286-C287 = C287-C288
 1.37 with sigma of 0.02
 C283-C288
 1.38 with sigma of 0.02
 C284-C285 = C285-C286
 1.36 with sigma of 0.02
 C273-C274 = C276-C271 = C271-C272
 1.37 with sigma of 0.02
 C273-C272
 1.38 with sigma of 0.02
 C274-C275 = C275-C276
 1.36 with sigma of 0.02
 C266-C267 = C269-C270 = C270-C265
 1.37 with sigma of 0.02
 C266-C265
 1.38 with sigma of 0.02
 C267-C268 = C268-C269
 1.36 with sigma of 0.02
 C11-C10 = C8-C7 = C7-C12
 1.37 with sigma of 0.02
 C11-C12
 1.38 with sigma of 0.02
 C289-C294 = C292-C291 = C291-C290
 1.37 with sigma of 0.02
 C289-C290
 1.38 with sigma of 0.02
 C10-C9 = C9-C8
 1.36 with sigma of 0.02
 C294-C293 = C293-C292
 1.36 with sigma of 0.02
 C277-C278 = C280-C281 = C281-C282
 1.37 with sigma of 0.02
 C277-C282
 1.38 with sigma of 0.02
 C278-C279 = C279-C280
 1.36 with sigma of 0.02
 C47-C43 = C43-C45 = C44-C46
 2.37 with sigma of 0.04
 C301-C303 = C303-C305 = C304-C306
 2.37 with sigma of 0.04
 C47-C45
 2.38 with sigma of 0.04
 C295-C297 = C297-C299 = C298-C300
 2.37 with sigma of 0.04
 C48-C44
 2.36 with sigma of 0.04
 C295-C299
 2.38 with sigma of 0.04
 C301-C305
 2.38 with sigma of 0.04
 C283-C285 = C285-C287 = C286-C288
 2.37 with sigma of 0.04
 C296-C298
 2.36 with sigma of 0.04
 C302-C304
 2.36 with sigma of 0.04
 C283-C287
 2.38 with sigma of 0.04
 C284-C286
 2.36 with sigma of 0.04
 C273-C275 = C275-C271 = C276-C272
 2.37 with sigma of 0.04
 C273-C271
 2.38 with sigma of 0.04
 C274-C276
 2.36 with sigma of 0.04
 C266-C268 = C268-C270 = C269-C265
 2.37 with sigma of 0.04
 C266-C270
 2.38 with sigma of 0.04
 C267-C269
 2.36 with sigma of 0.04
 C11-C9 = C9-C7 = C8-C12
 2.37 with sigma of 0.04
 C289-C293 = C293-C291 = C292-C290
 2.37 with sigma of 0.04
 C11-C7
 2.38 with sigma of 0.04
 C289-C291
 2.38 with sigma of 0.04
 C10-C8
 2.36 with sigma of 0.04
 C294-C292
 2.36 with sigma of 0.04
 C277-C279 = C279-C281 = C280-C282
 2.37 with sigma of 0.04
 C277-C281
 2.38 with sigma of 0.04
 C278-C280
 2.36 with sigma of 0.04
 C47-C48 \\sim C48-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C47
 with sigma of 0.02
 C47-C45 \\sim C47-C43 \\sim C45-C43 \\sim C44-C48 \\sim C44-C46 \\sim C46-C48
 with sigma of 0.04
 C295-C296 \\sim C296-C297 \\sim C297-C298 \\sim C298-C299 \\sim C299-C300
\\sim C300-C295
 with sigma of 0.02
 C301-C302 \\sim C302-C303 \\sim C303-C304 \\sim C304-C305 \\sim C305-C306
\\sim C306-C301
 with sigma of 0.02
 C283-C284 \\sim C284-C285 \\sim C285-C286 \\sim C286-C287 \\sim C287-C288
\\sim C288-C283
 with sigma of 0.02
 C295-C299 \\sim C295-C297 \\sim C299-C297 \\sim C298-C296 \\sim C298-C300
\\sim C300-C296
 with sigma of 0.04
 C283-C287 \\sim C283-C285 \\sim C287-C285 \\sim C286-C284 \\sim C286-C288
\\sim C288-C284
 with sigma of 0.04
 C301-C305 \\sim C301-C303 \\sim C305-C303 \\sim C304-C302 \\sim C304-C306
\\sim C306-C302
 with sigma of 0.04
 C273-C274 \\sim C274-C275 \\sim C275-C276 \\sim C276-C271 \\sim C271-C272
\\sim C272-C273
 with sigma of 0.02
 C273-C271 \\sim C273-C275 \\sim C271-C275 \\sim C276-C274 \\sim C276-C272
\\sim C272-C274
 with sigma of 0.04
 C266-C267 \\sim C267-C268 \\sim C268-C269 \\sim C269-C270 \\sim C270-C265
\\sim C265-C266
 with sigma of 0.02
 C266-C270 \\sim C266-C268 \\sim C270-C268 \\sim C269-C267 \\sim C269-C265
\\sim C265-C267
 with sigma of 0.04
 C11-C10 \\sim C10-C9 \\sim C9-C8 \\sim C8-C7 \\sim C7-C12 \\sim C12-C11
 with sigma of 0.02
 C11-C7 \\sim C11-C9 \\sim C7-C9 \\sim C8-C10 \\sim C8-C12 \\sim C12-C10
 with sigma of 0.04
 C289-C294 \\sim C294-C293 \\sim C293-C292 \\sim C292-C291 \\sim C291-C290
\\sim C290-C289
 with sigma of 0.02
 C289-C291 \\sim C289-C293 \\sim C291-C293 \\sim C292-C294 \\sim C292-C290
\\sim C290-C294
 with sigma of 0.04
 C277-C278 \\sim C278-C279 \\sim C279-C280 \\sim C280-C281 \\sim C281-C282
\\sim C282-C277
 with sigma of 0.02
 C277-C281 \\sim C277-C279 \\sim C281-C279 \\sim C280-C278 \\sim C280-C282
\\sim C282-C278
 with sigma of 0.04
 C289-C294 \\sim C1A-C1B
 with sigma of 0.02
 C289-C290 \\sim C1A-C1C
 with sigma of 0.02
 C294-C293 \\sim C1B-C1D
 with sigma of 0.02
 C293-C292 \\sim C1D-C1E
 with sigma of 0.02
 C292-C291 \\sim C1E-C1F
 with sigma of 0.02
 C291-C290 \\sim C1F-C1C
 with sigma of 0.02
 C289-C293 \\sim C1A-C1D
 with sigma of 0.04
 C289-C291 \\sim C1A-C1F
 with sigma of 0.04
 C294-C292 \\sim C1B-C1E
 with sigma of 0.04
 C294-C290 \\sim C1B-C1C
 with sigma of 0.04
 C293-C291 \\sim C1D-C1F
 with sigma of 0.04
 C292-C290 \\sim C1E-C1C
 with sigma of 0.04
4. Restrained planarity
 C43, C44, C45, C46, C47, C48
 with sigma of 0.1
 C302, C303, C304, C305, C306, C301
 with sigma of 0.1
 C283, C284, C285, C286, C287, C288
 with sigma of 0.1
 C299, C298, C297, C296, C295, C300
 with sigma of 0.1
 C271, C273, C274, C272, C275, C276
 with sigma of 0.1
 C266, C267, C268, C269, C270, C265
 with sigma of 0.1
 C7, C8, C9, C10, C11, C12
 with sigma of 0.1
 C291, C289, C294, C290, C293, C292
 with sigma of 0.1
 C279, C277, C278, C282, C281, C280
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C283 \\sim C284 \\sim C285 \\sim C286 \\sim C287 \\sim C288: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C302 \\sim C303 \\sim C304 \\sim C305 \\sim C306 \\sim C301: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C299 \\sim C298 \\sim C297 \\sim C296 \\sim C295 \\sim C300: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C271 \\sim C273 \\sim C274 \\sim C272 \\sim C275 \\sim C276: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C266 \\sim C267 \\sim C268 \\sim C269 \\sim C270 \\sim C265: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C291 \\sim C289 \\sim C294 \\sim C290 \\sim C293 \\sim C292: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C279 \\sim C277 \\sim C278 \\sim C282 \\sim C281 \\sim C280: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C297) \\sim Ueq, Uanis(C295) \\sim Ueq, Uanis(C296) \\sim Ueq,
Uanis(C300) \\sim Ueq, Uanis(C299) \\sim Ueq, Uanis(C298) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(C303) \\sim Ueq, Uanis(C301) \\sim Ueq, Uanis(C302) \\sim Ueq,
Uanis(C306) \\sim Ueq, Uanis(C305) \\sim Ueq, Uanis(C304) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
6. Rigid body (RIGU) restrains
 Au3, Au4, O3, O4, N5, N6, N7, N8, C67, C68, C69, C70, C71, C72, C73, C74, C75,
  C76, C77, C78, C79, C80, C81, C82, C83, C84, C85, C86, C87, C88, C89, C90,
 C91, C92, C93, C94, C95, C96, C97, C98, C99, C100, C101, C102, C103, C104,
 C105, C106, C107, C108, C109, C110, C111, C112, C113, C114, C115, C116, C118,
 C120, C119, C121, C122, C123, C124, C125, C126, C127, C128, C129, C130, C131,
 C132, C117
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C43, C44, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C283, C284, C285, C286, C287, C288
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Au1, Au2, O1, O2, N1, N2, N3, N4, C1, C2, C3, C4, C5, C6, C13, C14, C15, C16,
 C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32,
  C33, C34, C35, C36, C37, C38, C39, C40, C41, C42, C43, C44, C45, C46, C47,
 C48, C49, C50, C51, C52, C53, C54, C55, C56, C57, C58, C59, C60, C61, C62, C63,
  C64, C65, C66
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Au5, Au6, O5, O6, N9, N10, N11, N12, C133, C134, C135, C136, C137, C138, C172,
  C173, C174, C175, C176, C177, C178, C179, C180, C181, C183, C182, C184, C185,
 C186, C187, C192, C191, C190, C189, C188, C196, C197, C193, C194, C195, C139,
 C144, C142, C143, C141, C140, C145, C146, C147, C148, C149, C150, C151, C152,
 C153, C154, C156, C155, C157, C159, C158, C160, C161, C162, C163, C164, C165,
 C166, C167, C168, C169, C170, C171, C198
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Au7, Au8, O7, O8, N13, N14, N15, N16, C203, C199, C200, C201, C202, C204,
 C205, C206, C207, C208, C209, C210, C211, C212, C213, C214, C215, C216, C217,
 C218, C219, C220, C221, C222, C223, C225, C226, C227, C228, C229, C230, C231,
 C232, C234, C233, C235, C236, C237, C238, C239, C240, C241, C242, C243, C244,
 C245, C246, C247, C249, C248, C250, C252, C251, C253, C254, C255, C256, C257,
 C258, C259, C260, C261, C262, C264, C263, C224
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C302, C303, C304, C305, C306, C301
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C299, C298, C297, C296, C295, C300
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C271, C273, C274, C272, C275, C276
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C266, C267, C268, C269, C270, C265
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7, C8, C9, C10, C11, C12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C279, C277, C278, C282, C281, C280
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C1B, C1C, C1D, C1E, C1F
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C291, C289, C294, C290, C293, C292
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C291)=Sof(H291)=Sof(C289)=Sof(H289)=Sof(C294)=Sof(H294)=Sof(C290)=
 Sof(H290)=Sof(C293)=Sof(H293)=Sof(C292)=Sof(H292)=1-FVAR(1)
 Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1D)=
 Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1F)=FVAR(1)
 Fixed Sof: C302(0.5) H302(0.5) C303(0.5) H303(0.5) C304(0.5) H304(0.5)
 C305(0.5) H305(0.5) C306(0.5) H306(0.5) C301(0.5) H301(0.5) C299(0.5)
 H299(0.5) C298(0.5) H298(0.5) C297(0.5) H297(0.5) C296(0.5) H296(0.5)
 C295(0.5) H295(0.5) C300(0.5) H300(0.5)
8.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C34(H34), C37(H37), C49(H49), C52(H52), C61(H61),
 C64(H64), C181(H181), C184(H184), C196(H196), C193(H193), C154(H154),
 C157(H157), C166(H166), C169(H169), C88(H88), C91(H91), C100(H100), C103(H103),
  C115(H115), C118(H118), C127(H127), C130(H130), C220(H220), C223(H223),
 C232(H232), C235(H235), C247(H247), C250(H250), C259(H259), C262(H262)
8.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C18(H18),
 C19(H19), C20(H20), C30(H30), C31(H31), C32(H32), C41(H41), C42(H42), C45(H45),
  C46(H46), C47(H47), C57(H57), C58(H58), C59(H59), C173(H173), C174(H174),
 C177(H177), C178(H178), C179(H179), C191(H191), C190(H190), C189(H189),
 C144(H144), C142(H142), C143(H143), C141(H141), C140(H140), C146(H146),
 C147(H147), C150(H150), C151(H151), C152(H152), C162(H162), C163(H163),
 C164(H164), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C80(H80),
 C81(H81), C84(H84), C85(H85), C86(H86), C96(H96), C97(H97), C98(H98),
 C107(H107), C108(H108), C111(H111), C112(H112), C113(H113), C123(H123),
 C124(H124), C125(H125), C206(H206), C207(H207), C208(H208), C209(H209),
 C210(H210), C212(H212), C213(H213), C216(H216), C217(H217), C218(H218),
 C228(H228), C229(H229), C230(H230), C239(H239), C240(H240), C243(H243),
 C244(H244), C245(H245), C255(H255), C256(H256), C257(H257), C279(H279),
 C277(H277), C278(H278), C282(H282), C281(H281), C280(H280), C271(H271),
 C273(H273), C274(H274), C272(H272), C275(H275), C276(H276), C302(H302),
 C303(H303), C304(H304), C305(H305), C306(H306), C301(H301), C291(H291),
 C289(H289), C294(H294), C290(H290), C293(H293), C292(H292), C266(H266),
 C267(H267), C268(H268), C269(H269), C270(H270), C265(H265), C1A(H1A), C1B(H1B),
  C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F), C283(H283), C284(H284), C285(H285),
 C286(H286), C287(H287), C288(H288), C299(H299), C298(H298), C297(H297),
 C296(H296), C295(H295), C300(H300)
8.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,
 H26C), C27(H27A,H27B,H27C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C138(H13A,H13B,H13C),
 C183(H18A,H18B,H18C), C182(H18D,H18E,H18F), C185(H18G,H18H,H18I), C186(H18J,
 H18K,H18L), C197(H19A,H19B,H19C), C194(H19D,H19E,H19F), C195(H19G,H19H,H19I),
 C156(H15A,H15B,H15C), C155(H15D,H15E,H15F), C159(H15G,H15H,H15I), C158(H15J,
 H15K,H15L), C167(H16A,H16B,H16C), C168(H16D,H16E,H16F), C170(H17A,H17B,H17C),
 C171(H17D,H17E,H17F), C198(H19J,H19K,H19L), C72(H72A,H72B,H72C), C89(H89A,H89B,
 H89C), C90(H90A,H90B,H90C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C),
 C101(H10A,H10B,H10C), C102(H10D,H10E,H10F), C104(H10G,H10H,H10I), C105(H10J,
 H10K,H10L), C116(H11A,H11B,H11C), C120(H12A,H12B,H12C), C119(H11D,H11E,H11F),
 C128(H12D,H12E,H12F), C129(H12G,H12H,H12I), C131(H13D,H13E,H13F), C132(H13G,
 H13H,H13I), C117(H11G,H11H,H11I), C204(H20A,H20B,H20C), C221(H22A,H22B,H22C),
 C222(H22D,H22E,H22F), C225(H22G,H22H,H22I), C234(H23D,H23E,H23F), C233(H23G,
 H23H,H23I), C236(H23J,H23K,H23L), C237(H23M,H23N,H23O), C249(H24D,H24E,H24F),
 C248(H24G,H24H,H24I), C252(H25A,H25B,H25C), C251(H25D,H25E,H25F), C260(H26D,
 H26E,H26F), C261(H26G,H26H,H26I), C264(H26J,H26K,H26L), C263(H26M,H26N,H26O),
 C224(H22J,H22K,H22L)
;
_shelx_res_checksum              11206
_olex2_submission_special_instructions 'No special instructions were received'