Synthesis of 2,3-dihydroquinazolinimines and 1,3-diiminoisoindolines catalyzed by rare earth metal alkyl complexes through tandem addition/cyclization of nitriles with amines.
Guo, Dianjun; He, Jinqiang; Yuan, Qingbing; Zhou, Shuangliu; Zhu, Xiancui; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4484–4492; doi:10.1039/d5dt00106d

data_7718001
_publ_section_title
;
 Synthesis of 2,3-dihydroquinazolinimines and 1,3-diiminoisoindolines
 catalyzed by rare earth metal alkyl complexes through tandem
 addition/cyclization of nitriles with amines.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4484
_journal_page_last               4492
_journal_paper_doi               10.1039/d5dt00106d
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C49 H70 N5 Y'
_chemical_formula_sum            'C49 H70 N5 Y'
_chemical_formula_weight         818.01
_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   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2m3cgl
_audit_creation_date             2024-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-13 deposited with the CCDC.	2025-02-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.070(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5530(13)
_cell_length_b                   15.6876(16)
_cell_length_c                   27.880(3)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      22.579
_cell_measurement_theta_min      2.292
_cell_volume                     5435.9(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.998
_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  0.0735
_diffrn_reflns_av_unetI/netI     0.0767
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            46611
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.562
_diffrn_reflns_theta_min         1.965
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0992 before and 0.0432 after correction.
The Ratio of minimum to maximum transmission is 0.5168.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         12449
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.1281
_refine_ls_R_factor_gt           0.0664
_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^)+(0.0683P)^2^+3.8778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6884
_reflns_number_total             12449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00106d2.cif
_cod_data_source_block           8b
_cod_depositor_comments
'Adding full bibliography for 7717994--7718001.cif.'
_cod_original_cell_volume        5436.0(10)
_cod_database_code               7718001
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.793
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C35(H35), C28(H28), C1(H1), C47(H47), C9(H9)
4.b Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C20(H20A,H20B), C24(H24A,H24B), C23(H23A,H23B), C22(H22A,
 H22B), C21(H21A,H21B)
4.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C19(H19), C14(H14), C31(H31), C6(H6), C7(H7), C33(H33), C17(H17),
 C15(H15), C5(H5A), C32(H32), C16(H16), C44(H44), C45(H45), C43(H43)
4.d Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C3(H3A,H3B,H3C), C48(H48A,H48B,
 H48C), C37(H37A,H37B,H37C), C29(H29A,H29B,H29C), C2(H2A,H2B,H2C), C10(H10A,
 H10B,H10C), C41(H41A,H41B,H41C), C11(H11A,H11B,H11C), C49(H49A,H49B,H49C),
 C42(H42A,H42B,H42C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              8053
_shelx_fab_checksum              68953
_olex2_submission_special_instructions 'No special instructions were received'