The crystal and molecular structures of the nickel(II) complexes of malonamide-derived unsubstituted 14- and 13-membered tetraazamacrocycles and NMR study of the complexes in aqueous solution
Yaroslaw D. Lampeka; Sergey P. Gavrish; Robert W. Hay; Tanja Eisenblätter; Philip Lightfoot; J. Chem. Soc., Dalton Trans.  (2000) 2023–2029; doi:10.1039/b001510p

data_7009511
_publ_contact_author
;
    Dr Ya.D.Lampeka
    L.V.Pisarzhevskii Institute of Physical Chemistry
    National Academy of Sciences of Ukraine
    Prospekt Nauki 31, Kiev 03039, Ukraine
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_publ_section_title
;
 The crystal and molecular structures of the nickel(II) complexes of
 malonamide-derived unsubstituted 14- and 13-membered
 tetraazamacrocycles and NMR study of the complexes in aqueous solution
;
_journal_issue                   13
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              2023
_journal_page_last               2029
_journal_paper_doi               10.1039/b001510p
_journal_year                    2000
_chemical_formula_sum            'C9 H26 N4 Ni O7'
_chemical_formula_weight         361.03
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             'Tue Feb 15 15:40:54 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                94.48(2)
_cell_angle_beta                 102.43(2)
_cell_angle_gamma                83.95(3)
_cell_formula_units_Z            2
_cell_length_a                   9.892(3)
_cell_length_b                   11.279(4)
_cell_length_c                   7.352(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.2
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      24.2
_cell_volume                     795.3(4)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_diffrn_ambient_temperature      293.2
_diffrn_measurement_device       AFC7S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.07786
_diffrn_orient_matrix_UB_12      0.00191
_diffrn_orient_matrix_UB_13      0.11207
_diffrn_orient_matrix_UB_21      -0.05386
_diffrn_orient_matrix_UB_22      -0.04363
_diffrn_orient_matrix_UB_23      0.06961
_diffrn_orient_matrix_UB_31      0.04292
_diffrn_orient_matrix_UB_32      -0.07789
_diffrn_orient_matrix_UB_33      -0.04538
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  2.64
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2976
_diffrn_reflns_theta_max         25.02
_diffrn_standards_decay_%        -0.08
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.256
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       plate
_exptl_crystal_F_000             384.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.47
_refine_ls_extinction_coef       21.27434
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   2.909
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2535
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0407
_refine_ls_shift/esd_max         2.2520
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0398
_reflns_number_observed          2535
_reflns_number_total             2797
_reflns_observed_criterion       3.00
_cod_data_source_file            b001510p.txt
_cod_data_source_block           Lampeka_structure2
_cod_depositor_comments
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The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 47 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C9 H26 N4 O7 Ni '
_cod_database_code               7009511