Electronically and sterically varied tungsten carbonyls applied to the selective dearomatization of N-heteroarenes.
Bai, Pengtao; Liu, Yuzan; Fang, Li; Li, Ying; Wang, Jiahao; Cai, Yougen; Chen, Lei; Zhao, Jia-Jia; Song, Heng; Zong, Luyi; Xu, Chen; Dalton transactions (Cambridge, England : 2003) 55 (2026) 3454–3459; doi:10.1039/d6dt00164e

data_7720059
_publ_section_title
;
 Electronically and sterically varied tungsten carbonyls applied to the
 selective dearomatization of N-heteroarenes.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3454
_journal_page_last               3459
_journal_paper_doi               10.1039/d6dt00164e
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C37 H43 N3 O4 W, 2(C2 H3 N)'
_chemical_formula_sum            'C41 H49 N5 O4 W'
_chemical_formula_weight         859.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-03-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2026-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.9630(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1010(3)
_cell_length_b                   10.3729(2)
_cell_length_c                   28.2822(5)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.527
_cell_measurement_theta_min      2.439
_cell_volume                     4114.40(14)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            32151
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.545
_diffrn_reflns_theta_min         2.093
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    2.851
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       block
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.993
_refine_diff_density_min         -1.744
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.211
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9437
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.211
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0167P)^2^+4.5636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0619
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8160
_reflns_number_total             9437
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00164e2.cif
_cod_data_source_block           ywa_3_0m_pl
_cod_depositor_comments
'Adding full bibliography for 7720057--7720059.cif.'
_cod_original_cell_volume        4114.41(14)
_cod_database_code               7720059
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.744
_shelx_estimated_absorpt_t_min   0.360
_olex2_refinement_description
;
1.a Ternary CH refined with riding coordinates:
 C3(H3), C11(H11), C31(H31), C28(H28)
1.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C17(H17), C25(H25), C16(H16), C18(H18), C26(H26), C5(H5), C7(H7),
 C6(H6)
1.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C29(H29A,H29B,
 H29C), C33(H33A,H33B,H33C), C30(H30A,H30B,H30C), C10(H10A,H10B,H10C), C32(H32A,
 H32B,H32C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C)
;
_olex2_submission_special_instructions 'No special instructions were received'