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_7064081
_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         'Cl, C H2 Cl2, C27 H39 N2 O'
_chemical_formula_sum            'C28 H41 Cl3 N2 O'
_chemical_formula_weight         527.98
_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     dual
_audit_creation_date             2025-06-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.05.31 svn.r86d253d1 for OlexSys, GUI svn.r7254)
;
_audit_update_record
;
2025-06-18 deposited with the CCDC.	2025-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.149(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.818(5)
_cell_length_b                   17.701(8)
_cell_length_c                   15.614(8)
_cell_measurement_reflns_used    1013
_cell_measurement_temperature    120
_cell_measurement_theta_max      21.399
_cell_measurement_theta_min      2.30
_cell_volume                     2886(2)
_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      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2300
_diffrn_reflns_av_unetI/netI     0.2953
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24300
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.775
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5102
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1624 before and 0.1011 after correction.
The Ratio of minimum to maximum transmission is 0.5102.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0132(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         5643
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.2140
_refine_ls_R_factor_gt           0.0846
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.2241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2282
_reflns_number_total             5643
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03879k2.cif
_cod_data_source_block           a_CCDC4
_cod_depositor_comments
'Adding full bibliography for 7064076--7064082.cif.'
_cod_database_code               7064081
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.797
_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.a Ternary CH refined with riding coordinates:
 C10(H10), C13(H13), C22(H22), C25(H25)
2.b Secondary CH2 refined with riding coordinates:
 C1s(H1sa,H1sb), C2(H2a,H2b), C3(H3a,H3b)
2.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C14(H14a,H14b,H14c), C15(H15a,H15b,
 H15c), C23(H23a,H23b,H23c), C24(H24a,H24b,H24c), C26(H26a,H26b,H26c), C27(H27a,
 H27b,H27c)
;
_shelx_res_checksum              5962
_olex2_submission_special_instructions 'No special instructions were received'