Substituent changes in salen of CuIINaI-complexes to induce the various structure and catalytic activity towards 2-imidazolines from nitriles and 1,2-diaminopropane
Li, Quan-Quan; He, peng-xiu; Zhang, Jin; Zhang, Jidong; Xin, Yu Meng; Liu, Ping; Wang, Yao-Yu; Li, Jianli; Chemical Communications  (2019) –; doi:10.1039/C9CC00879A

data_7123161
_publ_section_title
;
 Substituent changes in salen of CuIINaI-complexes to induce the various
 structure and catalytic activity towards 2-imidazolines from nitriles and
 1,2-diaminopropane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC00879A
_journal_year                    2019
_chemical_formula_moiety         'C43 H52 Cu5 N22 Na2 O14, H2 O'
_chemical_formula_sum            'C43 H54 Cu5 N22 Na2 O15'
_chemical_formula_weight         1482.76
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2016-11-16
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-10-25 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                103.511(3)
_cell_angle_beta                 93.740(4)
_cell_angle_gamma                105.433(3)
_cell_formula_units_Z            1
_cell_length_a                   9.3751(18)
_cell_length_b                   12.984(3)
_cell_length_c                   13.416(3)
_cell_measurement_reflns_used    1509
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.57
_cell_measurement_theta_min      2.80
_cell_volume                     1516.4(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7848
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.489
_diffrn_reflns_theta_min         2.591
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.819
_exptl_absorpt_correction_T_max  0.635
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             753
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         5550
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1024
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1553
_refine_ls_wR_factor_ref         0.1843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3432
_reflns_number_total             5550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00879a2.cif
_cod_data_source_block           2
_cod_original_cell_volume        1516.4(5)
_cod_database_code               7123161
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O9-H9A
 0.85 with sigma of 0.01
 C22-H9A
 1.860653 with sigma of 0.02
 Na1-H9A
 3.033671 with sigma of 0.02
 O6-C20 \\sim C20-O6A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O9) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: O6(0.5) O7C(0.5) H7CA(0.5) H7CB(0.5) O8(0.5) H8A(0.5) H8B(0.5)
 C22(0.5) H22A(0.5) H22B(0.5) H22C(0.5) O9(0.5) H9A(0.5) O6A(0.5)
5.a Riding coordinates:
 O7C(H7CA,H7CB), O8(H8A,H8B), O9(H9A)
5.b Ternary CH refined with riding coordinates:
 C9(H9)
5.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C14(H14), C15(H15), C16(H16)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              12573
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'