Structural Changes upon Reduction of Dipyrido[2,3-a:3',2'-c]phenazine Probed by Vibrational Spectroscopy, ab Initio Calculations, and Deuteration Studies
Sarah L. Howell; Benjamin J. Matthewson; Matthew I. J. Polson; Anthony K. Burrell; Keith C. Gordon; Inorganic Chemistry 43 (2004) 2876–2887; doi:10.1021/ic030225l

data_4310893
_publ_section_title
;
 Structural Changes upon Reduction of Dipyrido[2,3-a:3',2'-c]phenazine
 Probed by Vibrational Spectroscopy, ab Initio Calculations, and
 Deuteration Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2876
_journal_page_last               2887
_journal_paper_doi               10.1021/ic030225l
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         'C91 H70 B2 Cl4 Cu2 F8 N4 O4 P4'
_chemical_formula_sum            'C91 H70 B2 Cl4 Cu2 F8 N4 O4 P4'
_chemical_formula_weight         1849.89
_chemical_name_systematic
;
?
;
_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                 97.2260(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.2590(1)
_cell_length_b                   21.1833(3)
_cell_length_c                   23.2960(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.12
_cell_volume                     8939.00(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'XPMA (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45563
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.9235
_exptl_absorpt_correction_T_min  0.8549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Blessing, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.11
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         15655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0944
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1169P)^2^+5.0143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.1961
_reflns_number_gt                10755
_reflns_number_total             15655
_reflns_threshold_expression     2sigma(I)
_cod_data_source_file            ic030225l_s2.cif
_cod_data_source_block           cu2ppb
_cod_original_cell_volume        8939.00(17)
_cod_database_code               4310893