Conformational rearrangement of 2,6-bis(1-salicyloylhydrazonoethyl)pyridine (H4daps) on complexation. Synthesis and X-ray characterisation of H4daps and its copper helicate complex [Cu(H2daps)(H2O)]2·2CH3CN
Manuel R. Bermejo; Rosa Pedrido; Ana M. González-Noya; María J. Romero; Miguel Vázquez; Lorenzo Sorace; New J. Chem. 27 (2003) 1753–1759; doi:10.1039/b305354g

data_7050636
_publ_section_title
;
 Conformational rearrangement of
 2,6-bis(1-salicyloylhydrazonoethyl)pyridine (H4daps) on complexation.
 Synthesis and X-ray characterisation of H4daps and its copper helicate
 complex [Cu(H2daps)(H2O)]2&#x00B7;2CH3CN
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1753
_journal_page_last               1759
_journal_paper_doi               10.1039/b305354g
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C23 H21 N5 O4'
_chemical_formula_weight         431.45
_chemical_name_common            H4DAPS
_chemical_name_systematic
;
H4DAPS
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.302(4)
_cell_length_b                   14.540(2)
_cell_length_c                   22.451(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      42.81
_cell_measurement_theta_min      22.8
_cell_volume                     4342(2)
_computing_cell_refinement       'CAD4-Express software (Nonius, 1994)'
_computing_data_collection       'CAD4-Express Software (Nonius, 1994)'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'MACH3 Enraf Nonius'
_diffrn_measurement_method       'omega/2 theta'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2389
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2896
_diffrn_reflns_theta_full        56.63
_diffrn_reflns_theta_max         56.63
_diffrn_reflns_theta_min         3.94
_diffrn_standards_interval_time  '120 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.767
_exptl_absorpt_correction_T_max  0.9412
_exptl_absorpt_correction_T_min  0.7097
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.227
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.873
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         2896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.2753
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1120
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                932
_reflns_number_total             2896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305354g.txt
_cod_data_source_block           2002be17
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7050636