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_4318981
_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_moiety         'C23 H23 Cu N5 O4'
_chemical_formula_sum            'C23 H23 Cu N5 O4'
_chemical_formula_weight         497.01
_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                104.44(4)
_cell_angle_beta                 104.94(5)
_cell_angle_gamma                103.58(4)
_cell_formula_units_Z            2
_cell_length_a                   8.576(4)
_cell_length_b                   11.143(6)
_cell_length_c                   12.990(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.42
_cell_measurement_theta_min      12.10
_cell_volume                     1100.6(10)
_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      0.043932
_diffrn_orient_matrix_UB_12      0.097740
_diffrn_orient_matrix_UB_13      0.026590
_diffrn_orient_matrix_UB_21      0.032312
_diffrn_orient_matrix_UB_22      0.001518
_diffrn_orient_matrix_UB_23      0.080098
_diffrn_orient_matrix_UB_31      0.115106
_diffrn_orient_matrix_UB_32      -0.003138
_diffrn_orient_matrix_UB_33      -0.001237
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0764
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6654
_diffrn_reflns_theta_full        29.96
_diffrn_reflns_theta_max         29.96
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.9997
_exptl_absorpt_correction_T_min  0.8481
_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 (Farrugia, J. Appl. Cryst. 32,
837-838, 1999).
Number of psi-scan sets used was   3
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         6392
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1389
_refine_ls_wR_factor_ref         0.1649
_reflns_number_gt                3445
_reflns_number_total             6392
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020127k_1.cif
_cod_data_source_block           Cu1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1100.6(9)
_cod_database_code               4318981
_exptl_absorpt_correction_t_ave  0.9577
_exptl_absorpt_rmerge_before     0.0102
_exptl_absorpt_rmerge_after      0.0102
_exptl_absorpt_theta_corr_max    1.0000
_exptl_absorpt_theta_corr_min    0.9992
_diffrn_standards_decay_corr_max 1.041
_diffrn_standards_decay_corr_min 0.960