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_7050637
_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            'C50 H48 Cu2 N12 O10'
_chemical_formula_weight         1104.08
_chemical_name_common            Cudaps
_chemical_name_systematic
;
Cudaps
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(3)
_cell_angle_beta                 129.566(3)
_cell_angle_gamma                90.000(3)
_cell_formula_units_Z            4
_cell_length_a                   23.936(4)
_cell_length_b                   14.650(2)
_cell_length_c                   18.069(3)
_cell_measurement_reflns_used    709
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.71
_cell_volume                     4884.5(13)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_molecular_graphics    'ORTEP-3 for windows (Farrugia, 1997)'
_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  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1033
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3521
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         1.77
_diffrn_standards_decay_%        'not significant'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.945639
_exptl_absorpt_correction_T_min  0.769207
_exptl_absorpt_correction_type   Sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         3521
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.600
_refine_ls_shift/su_mean         0.045
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1943
_reflns_number_gt                1759
_reflns_number_total             3521
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305354g.txt
_cod_data_source_block           be23rp1n
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_database_code               7050637