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_7705726
_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         'C35 H33 N5'
_chemical_formula_sum            'C35 H33 N5'
_chemical_formula_weight         523.69
_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'
_symmetry_Int_Tables_number      14
_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                 93.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.000(4)
_cell_length_b                   7.9196(16)
_cell_length_c                   19.361(4)
_cell_measurement_reflns_used    7552
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4737
_cell_measurement_theta_min      1.1340
_cell_volume                     2753.5(10)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9956
_diffrn_measured_fraction_theta_max 0.9956
_diffrn_measurement_details
;
scan:
	Number of images: 300
	           Slice: -110.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 40.0361
	          2theta: -19.9621
scan:
	Number of images: 270
	           Slice: -110.0000 - 25.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 40.0361
	          2theta: -19.9621
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0229
_diffrn_orient_matrix_UB_12      0.0413
_diffrn_orient_matrix_UB_13      0.0295
_diffrn_orient_matrix_UB_21      0.0267
_diffrn_orient_matrix_UB_22      0.0616
_diffrn_orient_matrix_UB_23      -0.1070
_diffrn_orient_matrix_UB_31      -0.0444
_diffrn_orient_matrix_UB_32      0.0264
_diffrn_orient_matrix_UB_33      0.0041
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0653
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18851
_diffrn_reflns_theta_full        27.4818
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.13
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6834
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.2632
_exptl_crystal_description       block
_exptl_crystal_F_000             1112.3898
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.4936
_refine_diff_density_min         -0.5855
_refine_diff_density_rms         0.0775
_refine_ls_d_res_high            0.7701
_refine_ls_d_res_low             17.9573
_refine_ls_goodness_of_fit_ref   1.0387
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    62
_refine_ls_number_parameters     361
_refine_ls_number_reflns         6284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0387
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+2.5717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1652
_refine_ls_wR_factor_ref         0.1746
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              10
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                5377
_reflns_number_total             6284
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d0dt03257c2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7705725--7705726.cif.'
_cod_original_cell_volume        2753.4(10)
_cod_database_code               7705726
_diffrn_number_total             6738
_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:
 C7(H7a,H7b), C35(H35a,H35b), C21(H21a,H21b), C28(H28a,H28b)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), N1(H1), C14(H14), N4(H4), C10(H10), C30(H30), C9(H9),
 C11(H11), C12(H12), C3(H3), C2(H2a), C23(H23), C33(H33), C31(H31), C5(H5a),
 C18(H18), C26(H26), C4(H4a), C16(H16), C17(H17), C19(H19), C32(H32), C24(H24),
 C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'