A New Branched Phenanthroline Derivative Ligand: Synthesis, Solution Chemistry, and Crystal Structures of Copper(II) and Zinc(II) Complexes
Gianluca Ambrosi; Mauro Formica; Vieri Fusi; Luca Giorgi; Annalisa Guerri; Mauro Micheloni; Paola Paoli; Roberto Pontellini; Patrizia Rossi; Inorganic Chemistry 46 (2007) 4737–4748; doi:10.1021/ic070184j

data_4308182
_publ_contact_author_address
;Institute of Chemical Sciences,
University of Urbino,
P.za Rinascimento 6, 
I-61029 Urbino, 
Italy
;
_publ_contact_author_email       vieri@uniurb.it
_publ_contact_author_fax         +390722350032
_publ_contact_author_name        'Vieri Fusi'
_publ_contact_author_phone       +390722378347
_publ_section_title
;
A New Branched Phenanthroline Derivative Ligand: Synthesis, Solution
Chemistry, and Crystal Structures of Copper(II) and Zinc(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4737
_journal_page_last               4748
_journal_paper_doi               10.1021/ic070184j
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C22 H36 Cu N8, 4(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C22 H42 Cl4 Cu N8 O19'
_chemical_formula_weight         927.98
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.837(5)
_cell_angle_beta                 80.571(6)
_cell_angle_gamma                85.084(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4067(7)
_cell_length_b                   9.6940(6)
_cell_length_c                   20.4120(10)
_cell_measurement_temperature    120
_cell_volume                     1792.4(2)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_computing_molecular_graphics    'ORTEP-3 (Farruggia, 1997)'
_computing_publication_material  'PARST97 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.4547
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'Xcalibur3 4 circles diffractometer'
_diffrn_measurement_method       'intensity from \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0760
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29194
_diffrn_reflns_theta_full        32.17
_diffrn_reflns_theta_max         32.17
_diffrn_reflns_theta_min         4.31
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.7052
_exptl_absorpt_correction_T_min  0.5892
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.2 (release 20-01-2006 CrysAlis171 .NET)
(compiled Jan 20 2006,12:36:28)
;
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             958
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         11315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.904
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                6626
_reflns_number_total             11315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070184j-file001_3.cif
_cod_data_source_block           5
_cod_original_cell_volume        1792.45(19)
_cod_database_code               4308182