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_7009510
_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            'C10 H30 N4 Ni O8'
_chemical_formula_weight         393.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Mon Jan 31 15:25:26 2000'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 92.17(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.247(2)
_cell_length_b                   24.982(4)
_cell_length_c                   9.436(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    473.2
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      25.0
_cell_volume                     1707.1(8)
_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      473.2
_diffrn_measurement_device       AFC7S
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_orient_matrix_UB_11      0.11940
_diffrn_orient_matrix_UB_12      0.01944
_diffrn_orient_matrix_UB_13      -0.00918
_diffrn_orient_matrix_UB_21      0.06855
_diffrn_orient_matrix_UB_22      -0.03453
_diffrn_orient_matrix_UB_23      0.01079
_diffrn_orient_matrix_UB_31      -0.00874
_diffrn_orient_matrix_UB_32      -0.00527
_diffrn_orient_matrix_UB_33      -0.10459
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.92
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3141
_diffrn_reflns_theta_max         25.00
_diffrn_standards_decay_%        -0.15
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       plate
_exptl_crystal_F_000             840.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.60
_refine_diff_density_min         -0.50
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   3.464
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         2286
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0476
_refine_ls_shift/esd_max         0.6660
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0541
_reflns_number_observed          2286
_reflns_number_total             2888
_reflns_observed_criterion       3.00
_cod_data_source_file            b001510p.txt
_cod_data_source_block           Ya
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_thermal_displace_type' tag value 'Uij' was replaced with
'Uani' value 53 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1707.1(7)
_cod_original_sg_symbol_H-M      'P 21/n     '
_cod_original_formula_sum        'C10 H30 N4 O8 Ni '
_cod_database_code               7009510