A case of alkylidyne-imine metathesis.
Yadav, Rinku; Ghiviriga, Ion; Abboud, Khalil K.; Veige, Adam S.; Chemical communications (Cambridge, England) 59 (2023) 12899–12902; doi:10.1039/d3cc04583h

data_7132295
_publ_section_title
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 A case of alkylidyne-imine metathesis.
;
_journal_issue                   86
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12899
_journal_page_last               12902
_journal_paper_doi               10.1039/d3cc04583h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C45 H49 N O2 W'
_chemical_formula_sum            'C45 H49 N O2 W'
_chemical_formula_weight         819.70
_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             2023-09-12
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
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2023-09-15 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                95.897(5)
_cell_angle_beta                 92.628(7)
_cell_angle_gamma                103.096(6)
_cell_formula_units_Z            2
_cell_length_a                   9.425(2)
_cell_length_b                   12.400(3)
_cell_length_c                   16.608(3)
_cell_measurement_reflns_used    9039
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.10
_cell_measurement_theta_min      2.21
_cell_volume                     1875.7(7)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_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  0.0553
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            90763
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.348
_diffrn_reflns_theta_min         1.980
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.117
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3725
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0785 before and 0.0573 after correction.
The Ratio of minimum to maximum transmission is 0.8641.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       plate
_exptl_crystal_F_000             832
_refine_diff_density_max         4.021
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         9366
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0256P)^2^+4.5283P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8548
_reflns_number_total             9366
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04583h2.cif
_cod_data_source_block           hkl_a
_cod_original_cell_volume        1875.8(7)
_cod_database_code               7132295
_shelx_shelxl_version_number     2019/3
_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
 C40-C45 \\sim C40-C45A
 with sigma of 0.02
 C40-C41 \\sim C40-C41A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 C40-C42 \\sim C40-C42A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C45A) = Uanis(C44A) = Uanis(C43A) = Uanis(C42A) = Uanis(C41A)
Uanis(C45) = Uanis(C44) = Uanis(C43) = Uanis(C42) = Uanis(C41)
4. Others
 Fixed Sof: C41A(0.55) H41A(0.55) C42A(0.55) H42A(0.55) C43A(0.55) H43A(0.55)
 C44A(0.55) H44A(0.55) C45A(0.55) H45A(0.55) C45(0.45) H45(0.45) C41(0.45)
 H41(0.45) C42(0.45) H42(0.45) C44(0.45) H44(0.45) C43(0.45) H43(0.45)
5.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C5(H5), C8(H8), C4(H4), C3(H3), C14(H14), C9(H9),
 C15(H15), C16(H16), C33(H33), C41A(H41A), C42A(H42A), C43A(H43A), C44A(H44A),
 C45A(H45A), C29(H29), C32(H32), C31(H31), C30(H30), C45(H45), C41(H41),
 C42(H42), C44(H44), C43(H43)
5.c Fitted hexagon refined as free rotating group:
 C40(C41A,C42A,C43A,C44A,C45A)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C38(H38A,H38B,H38C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C)
;
_shelx_res_checksum              282
_olex2_submission_special_instructions 'No special instructions were received'