Expanded ring 1,3,5-oxadiazinan-4-ylidene complexes: synthesis and catalysis
Isaeva, Dilshodakhon K.; Topchiy, Maxim A.; Drokin, Egor A.; Rasskazova, Mariya A.; Minaeva, Lidiya I.; Smol’yakov, Alexander F.; Asachenko, Andrey F.; New Journal of Chemistry 49 (2025) 20073–20080; doi:10.1039/D5NJ03879K

data_7064078
_publ_section_title
;
 Expanded ring 1,3,5-oxadiazinan-4-ylidene complexes: synthesis and
 catalysis
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20073
_journal_page_last               20080
_journal_paper_doi               10.1039/D5NJ03879K
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C27 H38 Au Cl N2 O, 0.5(C2 H4 Cl4)'
_chemical_formula_sum            'C28 H40 Au Cl3 N2 O'
_chemical_formula_weight         723.93
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-05-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-06-18 deposited with the CCDC.	2025-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2856(3)
_cell_length_b                   15.7171(5)
_cell_length_c                   23.3139(9)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.218
_cell_measurement_theta_min      2.62
_cell_volume                     3036.07(19)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0365
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            27166
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.592
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.132
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1349 before and 0.0516 after correction.
The Ratio of minimum to maximum transmission is 0.3456.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.546
_refine_diff_density_min         -1.316
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0258
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+2.6884P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0470
_refine_ls_wR_factor_ref         0.0480
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2803
_reflns_number_total             3055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03879k2.cif
_cod_data_source_block           a_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7064076--7064082.cif.'
_cod_database_code               7064078
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.534
_shelx_estimated_absorpt_t_min   0.274
_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. Others
 Fixed Sof: Cl1R(0.5) Cl2S(0.5) H1SA(0.5) H1SB(0.5)
3.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C)
;
_shelx_res_checksum              57290
_olex2_submission_special_instructions 'No special instructions were received'