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_7057558
_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 H38 N4 Ni O2'
_chemical_formula_weight         521.33
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-06-11 deposited with the CCDC.
2018-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.104(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0046(13)
_cell_length_b                   8.5202(9)
_cell_length_c                   26.095(2)
_cell_measurement_reflns_used    2700
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.2960
_cell_measurement_theta_min      2.5060
_cell_volume                     2667.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.0303
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0746
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            14110
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.425
_diffrn_reflns_theta_min         1.842
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'reddish brown'
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.285
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         6171
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.2704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1357
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3577
_reflns_number_total             6171
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj01718b2.cif
_cod_data_source_block           rgs11a
_cod_depositor_comments
'Adding full bibliography for 7057557--7057558.cif.'
_cod_database_code               7057558
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              6672