Aza-crown compounds synthesised by the self-condensation of 2-amino-benzyl alcohol over a pincer ruthenium catalyst and applied in the transfer hydrogenation of ketones.
Zhang, Shanshan; Wang, Zheng; Cao, Qianrong; Yue, Erlin; Liu, Qingbin; Ma, Yanping; Liang, Tongling; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15821–15827; doi:10.1039/d0dt03257c

data_7705725
_publ_section_title
;
 Aza-crown compounds synthesised by the self-condensation of
 2-amino-benzyl alcohol over a pincer ruthenium catalyst and applied in
 the transfer hydrogenation of ketones.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15821
_journal_page_last               15827
_journal_paper_doi               10.1039/d0dt03257c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C21 H21 N3'
_chemical_formula_sum            'C21 H21 N3'
_chemical_formula_weight         315.41
_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   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-06-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-08 deposited with the CCDC.	2020-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.60(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.8540(10)
_cell_length_b                   21.542(4)
_cell_length_c                   15.408(3)
_cell_measurement_reflns_used    5276
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4622
_cell_measurement_theta_min      1.3229
_cell_volume                     1609.5(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22322
_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         27.478
_diffrn_reflns_theta_min         1.626
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.9940
_exptl_absorpt_correction_T_min  0.9896
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.134
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.556
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3689
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0623P)^2^+1.2038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3542
_reflns_number_total             3689
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03257c2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7705725--7705726.cif.'
_cod_original_cell_volume        1609.5(6)
_cod_database_code               7705725
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.990
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C14(H14A,H14B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N2(H2), C2(H2A), C18(H18), C19(H19), C16(H16), C3(H3A),
 C5(H5), C9(H9), C17(H17), C4(H4), C11(H11), C12(H12), C10(H10)
;
_shelx_res_checksum              38366
_olex2_submission_special_instructions 'No special instructions were received'