A New Chiral N,N',O-Donor Heteroscorpionate Ligand. Structures of Ni2+, Cu2+, Zn2+ Complexes and Study of Solution Equilibria by Means of 1H NMR/UV-Vis Titrations and EXSY NMR Spectroscopy
Marcello Gennari; Matteo Tegoni; Maurizio Lanfranchi; Maria Angela Pellinghelli; Luciano Marchiò; Inorganic Chemistry 46 (2007) 3367–3377; doi:10.1021/ic062228e

data_4307734
_publ_contact_author
;
     Dr. Luciano Marchi\`o
     Dip. Chimica Generale ed Inorganica, Chimica Analitica,
     Chimica Fisica. V.le G.P. Usberti 17/a. Parma. Italy
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_publ_contact_author_email       marchio@unipr.it
_publ_contact_author_fax         '+39 0521 905557'
_publ_contact_author_phone       '+39 0521 905424'
_publ_section_title
;
A New Chiral N,N',O-Donor Heteroscorpionate Ligand. Structures of Ni2+,
Cu2+, Zn2+ Complexes and Study of Solution Equilibria by Means of 1H
NMR/UV-Vis Titrations and EXSY NMR Spectroscopy
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3367
_journal_page_last               3377
_journal_paper_doi               10.1021/ic062228e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C12 h15 Cl2 N3 O Zn'
_chemical_formula_sum            'C12 H15 Cl2 N3 O Zn'
_chemical_formula_weight         353.54
_chemical_name_systematic
;
 ?
;
_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                90.00
_cell_angle_beta                 116.380(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.888(2)
_cell_length_b                   14.9470(10)
_cell_length_c                   14.4180(10)
_cell_measurement_reflns_used    8837
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      1.86
_cell_volume                     3453.5(5)
_computing_cell_refinement       Saint
_computing_data_collection       Smart
_computing_data_reduction        Saint
_computing_molecular_graphics    'Ortep3 for windows'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Sir97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker Smart 1000 area detector'
_diffrn_measurement_method       'Theta&omega scan'
_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  0.0366
_diffrn_reflns_av_sigmaI/netI    0.0300
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18536
_diffrn_reflns_theta_full        28.02
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.727
_exptl_absorpt_correction_T_max  0.409
_exptl_absorpt_correction_T_min  1.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         3950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                2682
_reflns_number_total             3950
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062228esi20061123_043721_1.cif
_cod_data_source_block           mg210
_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 
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_cod_database_code               4307734