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_7064082
_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         'C36 H47 Cl N2 O Pd, C4 H10 O'
_chemical_formula_sum            'C40 H57 Cl N2 O2 Pd'
_chemical_formula_weight         739.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-09
_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                 95.704(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1124(10)
_cell_length_b                   14.6094(10)
_cell_length_c                   17.3407(12)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.520
_cell_measurement_theta_min      2.361
_cell_volume                     3809.6(4)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            51864
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.826
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.592
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1191 before and 0.0446 after correction.
The Ratio of minimum to maximum transmission is 0.7865.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       plate
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.706
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         7482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0247
_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^)+(0.0299P)^2^+3.0762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0658
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6698
_reflns_number_total             7482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03879k2.cif
_cod_data_source_block           ID-164-fr2
_cod_depositor_comments
'Adding full bibliography for 7064076--7064082.cif.'
_cod_database_code               7064082
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.756
_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: C2(0.75) H2(0.75) C2R(0.25) H2R(0.25) C3(0.75) H3(0.75) C3R(0.25)
 H3R(0.25)
3.a Ternary CH refined with riding coordinates:
 C2(H2), C3(H3), C3R(H3R), C19(H19), C22(H22), C31(H31), C34(H34)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3S(H3SA,H3SB)
3.c Aromatic/amide H refined with riding coordinates:
 C2R(H2R), C9(H9), C5(H5), C6(H6), C7(H7), C8(H8), C15(H15), C16(H16),
 C17(H17), C27(H27), C28(H28), C29(H29)
3.d Fitted hexagon refined as free rotating group:
 C9(C4,C5,C6,C7,C8)
3.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C1S(H1SA,H1SB,H1SC), C4S(H4SA,H4SB,H4SC)
;
_shelx_res_checksum              74293
_olex2_submission_special_instructions 'No special instructions were received'