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_7123160
_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_sum            'C76 H82 Cu8 N38 Na4 O22'
_chemical_formula_weight         2480.08
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.150(3)
_cell_length_b                   17.374(2)
_cell_length_c                   26.768(3)
_cell_measurement_reflns_used    4020
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      18.52
_cell_measurement_theta_min      2.34
_cell_volume                     9836(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0895
_diffrn_reflns_av_unetI/netI     0.0772
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            50919
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.110
_diffrn_reflns_theta_min         2.149
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.801
_exptl_absorpt_correction_T_max  0.637
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.923
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     691
_refine_ls_number_reflns         9739
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0418P)^2^+6.6044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1235
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5217
_reflns_number_total             9739
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc00879a2.cif
_cod_data_source_block           1
_cod_depositor_comments
;

2023-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C38 H41 Cu4 N19 Na2 O11'
_cod_original_formula_weight         1240.04
_cod_original_formula_moiety         'C38 H41 Cu4 N19 Na2 O11'
_cod_original_formula_units_Z            8
_cod_database_code               7123160
_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,H) groups
2. Restrained distances
 N6-N7
 1.1 with sigma of 0.001
 N6-N5
 1.1 with sigma of 0.001
 N5-N7
 2.2 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cu3, N5, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7, N7A, N6, N5A, N5, Cu3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N7A, N7, N6, N5, N5A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N7A)=Sof(N5A)=1-FVAR(1)
 Sof(N5)=Sof(N7)=FVAR(1)
6.a Riding coordinates:
 O9(H9A,H9B)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9C,H9D), C10(H10A,H10B), C27(H27A,H27B), C28(H28A,H28B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C13(H13), C14(H14), C15(H15),
 C21(H21), C22(H22), C23(H23), C26(H26), C29(H29), C31(H31), C32(H32), C33(H33)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C36(H36A,H36B,
 H36C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              14477
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'