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_7717994
_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         'C33 H56 Gd N3 Si2'
_chemical_formula_sum            'C33 H56 Gd N3 Si2'
_chemical_formula_weight         708.23
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2m3cch
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6951(5)
_cell_length_b                   16.8616(8)
_cell_length_c                   20.6165(10)
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    297.3
_cell_measurement_theta_max      26.110
_cell_measurement_theta_min      2.316
_cell_volume                     3717.9(3)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      297.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43783
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         1.560
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.871
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1188 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.6037. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       block
_exptl_crystal_F_000             1468
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 3010 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         8520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0276
_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^)+(0.0201P)^2^+0.5814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                7569
_reflns_number_total             8520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00106d2.cif
_cod_data_source_block           1a
_cod_depositor_comments
'Adding full bibliography for 7717994--7718001.cif.'
_cod_database_code               7717994
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.684
_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:
 C1(H1), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C30(H30a,H30b), C26(H26a,H26b), C25(H25a,H25b), C22(H22a,H22b), C24(H24a,
 H24b), C23(H23a,H23b), C20(H20a,H20b), C21(H21a,H21b)
2.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C5(H5), C19(H19), C7(H7), C6(H6), C17(H17), C15(H15), C16(H16)
2.d Idealised Me refined as rotating group:
 C31(H31a,H31b,H31c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C11(H11a,H11b,
 H11c), C28(H28a,H28b,H28c), C2(H2a,H2b,H2c), C10(H10a,H10b,H10c), C29(H29a,
 H29b,H29c), C27(H27a,H27b,H27c), C3(H3a,H3b,H3c)
;
_shelx_res_checksum              80825
_olex2_submission_special_instructions 'No special instructions were received'