Polyamine Macrocycles Incorporating a Phenanthroline Unit: Their Synthesis, Basicity, and Cu(II) Coordination
Carla Bazzicalupi; Andrea Bencini; Vieri Fusi; Claudia Giorgi; Piero Paoletti; Barbara Valtancoli; Inorganic Chemistry 37 (1998) 941–948; doi:10.1021/ic9708428

data_4322692
_publ_section_title
;
 Polyamine Macrocycles Incorporating a Phenanthroline Unit: Their
 Synthesis, Basicity, and Cu(II) Coordination
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              941
_journal_page_last               948
_journal_paper_doi               10.1021/ic9708428
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety
;
Cu 2+, C27 H 39 N7 2+, (S C N 1-)2, (Cl O4 -1)2, (H2 O)3
;
_chemical_formula_structural
;
(Cu) (C27 H39 N7) (S C N)2 (Cl O4)2 (H2 O)3
;
_chemical_formula_sum            'C29 H45 Cl2 Cu N9 O11 S2'
_chemical_formula_weight         894.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                106.87(3)
_cell_angle_beta                 90.22(8)
_cell_angle_gamma                104.48(8)
_cell_formula_units_Z            2
_cell_length_a                   9.770(10)
_cell_length_b                   12.027(5)
_cell_length_c                   18.006(7)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      9.56
_cell_measurement_theta_min      5.10
_cell_volume                     1954(2)
_computing_cell_refinement       'ENRAF-NONIUS CAD4'
_computing_data_collection       'ENRAF-NONIUS CAD4'
_computing_data_reduction        'ENRAF-NONIUS CAD4'
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'PARST93 (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'Patterson method'
_diffrn_ambient_temperature      298
_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  0.0852
_diffrn_reflns_av_sigmaI/netI    0.2311
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3804
_diffrn_reflns_theta_max         20.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.870
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'Walker and Stuart, 1983'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             930
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.055
_refine_ls_goodness_of_fit_obs   1.252
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         3646
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_restrained_S_obs      1.252
_refine_ls_R_factor_all          0.2313
_refine_ls_R_factor_obs          0.0971
_refine_ls_shift/esd_max         0.679
_refine_ls_shift/esd_mean        0.109
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+7.9685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2553
_refine_ls_wR_factor_obs         0.1832
_reflns_number_observed          1620
_reflns_number_total             3648
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9708428.cif
_cod_data_source_block           '[H2LCu(SCN)2].(ClO4)2.3H2O'
_cod_original_cell_volume        1953.7(23)
_cod_database_code               4322692