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_7132296
_publ_section_title
;
 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         'C44 H47 N O2 W'
_chemical_formula_sum            'C44 H47 N O2 W'
_chemical_formula_weight         805.67
_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             2023-08-31
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-09-15 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                101.4590(10)
_cell_angle_beta                 91.8750(10)
_cell_angle_gamma                99.739(2)
_cell_formula_units_Z            2
_cell_length_a                   9.3557(5)
_cell_length_b                   11.8178(5)
_cell_length_c                   16.8483(9)
_cell_measurement_reflns_used    9685
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.38
_cell_volume                     1795.12(16)
_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 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0497
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76986
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.538
_diffrn_reflns_theta_min         1.951
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.255
_exptl_absorpt_correction_T_max  0.4311
_exptl_absorpt_correction_T_min  0.3922
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0717 before and 0.0584 after correction.
The Ratio of minimum to maximum transmission is 0.9098.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       plate
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         9050
_refine_ls_number_restraints     404
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0174P)^2^+1.2817P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0434
_refine_ls_wR_factor_ref         0.0452
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8223
_reflns_number_total             9050
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc04583h2.cif
_cod_data_source_block           hkl
_cod_database_code               7132296
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.792
_shelx_estimated_absorpt_t_min   0.226
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C14(H14), C16(H16), C15(H15), C29(H29), C40(H40), C10(H10), C8(H8),
 C33(H33), C44(H44), C5(H5), C32(H32), C3(H3), C9(H9), C4(H4), C41(H41),
 C31(H31), C43(H43), C30(H30), C42(H42)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C), C21(H21A,H21B,H21C), C38(H38A,H38B,
 H38C), C22(H22A,H22B,H22C), C37(H37A,H37B,H37C), C36(H36A,H36B,H36C), C24(H24A,
 H24B,H24C), C20(H20A,H20B,H20C)
;
_shelx_res_checksum              19124
_olex2_submission_special_instructions 'No special instructions were received'