Synthesis and characterization of regioselective substituted tetrapyridophenazine ligands and their Ru(II) complexes.
Karnahl, Michael; Tschierlei, Stefanie; Kuhnt, Christian; Dietzek, Benjamin; Schmitt, Michael; Popp, Jürgen; Schwalbe, Matthias; Krieck, Sven; Görls, Helmar; Heinemann, Frank W.; Rau, Sven; Dalton transactions (Cambridge, England : 2003) 39 (2010) 2359–2370; doi:10.1039/b917484b

data_7024472
_publ_section_title
;
 Synthesis and characterization of regioselective substituted
 tetrapyridophenazine ligands and their Ru(II) complexes.
;
_journal_issue                   9
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2359
_journal_page_last               2370
_journal_paper_doi               10.1039/b917484b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C60 H58 Br2 N10 Ru, 2.0(F6 P)'
_chemical_formula_sum            'C60 H58 Br2 F12 N10 P2 Ru'
_chemical_formula_weight         1469.99
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.624(6)
_cell_angle_beta                 74.766(4)
_cell_angle_gamma                75.583(8)
_cell_formula_units_Z            2
_cell_length_a                   15.6539(14)
_cell_length_b                   15.9733(16)
_cell_length_c                   16.3583(6)
_cell_measurement_reflns_used    237
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      6.00
_cell_volume                     3748.4(5)
_computing_cell_refinement       'EVALCCD (Duisenberg, 2003)'
_computing_data_collection       'COLLECT (Bruker-Nonius, 2002)'
_computing_data_reduction        'EVALCCD (Duisenberg, 2003)'
_computing_molecular_graphics    'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_publication_material  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_refinement  'SHELXTL 6.12 (Bruker AXS, 2002)'
_computing_structure_solution    'SHELXTL 6.12 (Bruker AXS, 2002)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method
;
\f- and \w-rotations with 2.00 \% and 120 sec per frame
;
_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  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            80953
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    1.387
_exptl_absorpt_correction_T_max  0.800
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
;
_refine_diff_density_max         2.122
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.301
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         13207
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.319
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0843
_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^)+(0.1127P)^2^+5.2350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2267
_refine_ls_wR_factor_ref         0.2487
_reflns_number_gt                8609
_reflns_number_total             13207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b917484b.txt
_cod_data_source_block           mk0802sq
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7024472