Polyamine Macrocycles Incorporating a Phenolic Function: Their Synthesis, Basicity, and Coordination Behavior toward Metal Cations. Crystal Structure of a Binuclear Nickel Complex
Paolo Dapporto; Mauro Formica; Vieri Fusi; Mauro Micheloni; Paola Paoli; Roberto Pontellini; Paolo Romani; Patrizia Rossi; Inorganic Chemistry 39 (2000) 2156–2163; doi:10.1021/ic991291j

data_4320943
_publ_contact_author
;
    Vieri Fusi
 Instutute of Chemical Sciences, University of Urbino, P.za Rinascimento 6,
 I-61029, Urbino, Italy
;
_publ_contact_author_email       vieri@chim.uniurb.it
_publ_section_title
;
 Polyamine Macrocycles Incorporating a Phenolic Function: Their Synthesis,
 Basicity, and Coordination Behavior toward Metal Cations. Crystal
 Structure of a Binuclear Nickel Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2156
_journal_page_last               2163
_journal_paper_doi               10.1021/ic991291j
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety
;
(Ni 2+)2, C16 H28 N5 O 1-, (Cl -1)3, (H2 O)3, C H4 O
;
_chemical_formula_structural
'(Ni)2 (C16 H28 N5 O1) (Cl)3 (H2 O)3 (C H4 O)'
_chemical_formula_sum            'C17 H38 Cl3 N5 Ni2 O2'
_chemical_formula_weight         568.25
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.821(5)
_cell_length_b                   10.270(4)
_cell_length_c                   17.663(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.3
_cell_measurement_theta_min      8.5
_cell_volume                     2544.0(16)
_computing_cell_refinement       'CAD4 Enraf Nonius'
_computing_data_collection       'CAD4 Enraf Nonius'
_computing_data_reduction        'CAD4 Enraf Nonius'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'PARST93 (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR97 (Altomare, 1994)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'ENRAF NONIUS CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0881
_diffrn_reflns_av_sigmaI/netI    0.2071
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2451
_diffrn_reflns_theta_max         19.96
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.832
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.28
_exptl_absorpt_correction_type   'refdelf (Walker and Stuart, 1983)'
_exptl_crystal_colour            pale_green
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.050
_refine_ls_goodness_of_fit_obs   1.193
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     201
_refine_ls_number_reflns         2350
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_restrained_S_obs      1.193
_refine_ls_R_factor_all          0.2031
_refine_ls_R_factor_obs          0.0973
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2794
_refine_ls_wR_factor_obs         0.2136
_reflns_number_observed          1160
_reflns_number_total             2354
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic991291j.cif
_cod_data_source_block           Ni2(LOH)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1187P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4320943