Synthesis, Structure, and Second-Order Nonlinear Optical Properties of Copper(II) and Palladium(II) Acentric Complexes with N-Salicylidene-N'-aroylhydrazine Tridentate Ligands
F. Cariati; U. Caruso; R. Centore; W. Marcolli; A. De Maria; B. Panunzi; A. Roviello; A. Tuzi; Inorganic Chemistry 41 (2002) 6597–6603; doi:10.1021/ic020127k

data_4318983
_publ_section_title
;
 Synthesis, Structure, and Second-Order Nonlinear Optical Properties of
 Copper(II) and Palladium(II) Acentric Complexes with
 N-Salicylidene-N'-aroylhydrazine Tridentate Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6597
_journal_page_last               6603
_journal_paper_doi               10.1021/ic020127k
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C36 H34 Cu N6 O4'
_chemical_formula_weight         678.23
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.77(2)
_cell_angle_beta                 77.98(2)
_cell_angle_gamma                70.663(10)
_cell_formula_units_Z            4
_cell_length_a                   12.219(2)
_cell_length_b                   13.8305(10)
_cell_length_c                   20.948(6)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.72
_cell_measurement_theta_min      11.92
_cell_volume                     3264.2(11)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega scans'
_diffrn_orient_matrix_type
;
    x-axis points to radiation source
    the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.031032
_diffrn_orient_matrix_UB_12      -0.076315
_diffrn_orient_matrix_UB_13      -0.002674
_diffrn_orient_matrix_UB_21      0.072243
_diffrn_orient_matrix_UB_22      -0.001097
_diffrn_orient_matrix_UB_23      0.015784
_diffrn_orient_matrix_UB_31      -0.040027
_diffrn_orient_matrix_UB_32      -0.007524
_diffrn_orient_matrix_UB_33      0.046137
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.1671
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16125
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.56
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        4
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.718
_exptl_absorpt_correction_T_max  0.9995
_exptl_absorpt_correction_T_min  0.9505
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst.
A24, 351 as implemented in WinGX program (Farrugia, J. Appl. Cryst.
32, 837-838, 1999).
Number of psi-scan sets used was   2
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     847
_refine_ls_number_reflns         15702
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.2394
_refine_ls_R_factor_gt           0.0682
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1879
_reflns_number_gt                5806
_reflns_number_total             15702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020127k_3.cif
_cod_data_source_block           Cu2*
_cod_database_code               4318983
_exptl_absorpt_correction_t_ave  0.9748
_exptl_absorpt_rmerge_before     0.0113
_exptl_absorpt_rmerge_after      0.0113
_exptl_absorpt_theta_corr_max    1.0000
_exptl_absorpt_theta_corr_min    0.9993
_diffrn_standards_decay_corr_max 1.066
_diffrn_standards_decay_corr_min 0.978