Synthesis and crystal structures of salen-type Cu(ii) and Ni(ii) Schiff base complexes: application in [3+2]-cycloaddition and A3-coupling reactions
Agrahari, Bhumika; Layek, Samaresh; Ganguly, Rakesh; Pathak, Devendra D.; New Journal of Chemistry 42 (2018) 13754–; doi:10.1039/C8NJ01718B

data_7057557
_publ_section_title
;
 Synthesis and crystal structures of salen-type Cu(ii) and Ni(ii) Schiff
 base complexes: application in [3+2]-cycloaddition and A3-coupling
 reactions
;
_journal_issue                   16
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              13754
_journal_paper_doi               10.1039/C8NJ01718B
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C28 H39 Cu N4 O2.5'
_chemical_formula_weight         535.17
_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_method           SHELXL-2014/7
_audit_update_record
;
2017-09-26 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                92.716(3)
_cell_angle_beta                 93.956(3)
_cell_angle_gamma                102.009(3)
_cell_formula_units_Z            4
_cell_length_a                   9.4610(11)
_cell_length_b                   15.3673(17)
_cell_length_c                   19.021(2)
_cell_measurement_reflns_used    2873
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      22.52
_cell_measurement_theta_min      2.47
_cell_volume                     2693.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.976
_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  0.1046
_diffrn_reflns_av_unetI/netI     0.1956
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20273
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.173
_diffrn_reflns_theta_min         1.357
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.46
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.919
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         10518
_refine_ls_number_restraints     239
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.1722
_refine_ls_R_factor_gt           0.0709
_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^)+(0.0614P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1363
_refine_ls_wR_factor_ref         0.1721
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4845
_reflns_number_total             10518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01718b2.cif
_cod_data_source_block           rgdp22
_cod_depositor_comments
'Adding full bibliography for 7057557--7057558.cif.'
_cod_original_formula_sum        'C28 H39 Cu N4 O2.50'
_cod_database_code               7057557
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.718
_shelx_estimated_absorpt_t_max   0.936
_shelx_res_checksum              59780