Molecular and Electronic Structures of Complexes Containing 1-(2-pyridylazo)-2-phenanthrol (PAPL): Revisiting a Redox-Active Ligand
Natasha Van Damme; Alan J. Lough; Serge I. Gorelsky; Martin T. Lemaire; Inorganic Chemistry 52 (2013) 13021–13028; doi:10.1021/ic401618u

data_4336709
_publ_section_title
;
 Molecular and Electronic Structures of Complexes Containing
 1-(2-pyridylazo)-2-phenanthrol (PAPL): Revisiting a Redox-Active Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13021
_journal_page_last               13028
_journal_paper_doi               10.1021/ic401618u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C38 H24 N6 O2 Zn, C4 H10 O'
_chemical_formula_sum            'C42 H34 N6 O3 Zn'
_chemical_formula_weight         736.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 119.539(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1546(12)
_cell_length_b                   22.634(2)
_cell_length_c                   13.0599(11)
_cell_measurement_reflns_used    9868
_cell_measurement_temperature    147(2)
_cell_measurement_theta_max      66.38
_cell_measurement_theta_min      3.86
_cell_volume                     3383.0(5)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      147(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker Kappa APEX-DUO CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multi-layer optics'
_diffrn_radiation_source         'Bruker ImuS'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22567
_diffrn_reflns_theta_full        66.43
_diffrn_reflns_theta_max         66.43
_diffrn_reflns_theta_min         3.86
_exptl_absorpt_coefficient_mu    1.423
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.6837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       needle
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.841
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         5823
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0420P)^2^+3.3553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0934
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                5493
_reflns_number_total             5823
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic401618u_si_001.cif
_cod_data_source_block           d12279
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4336709