Synthesis of 4,5-diheteroarylphenanthrenes and their dinuclear ruthenium(ii) bis(2,2′:6′,2″-terpyridine) complexes possessing severe helical twists
Wen, Bo; Petersen, Jeffrey L.; Wang, Kung K.; Chemical Communications 46 (2010) 1938–1940; doi:10.1039/b921667g

data_7111565
_publ_section_title
;
 Synthesis of 4,5-diheteroarylphenanthrenes and their dinuclear
 ruthenium(ii) bis(2,2&#x2032;:6&#x2032;,2&#x2033;-terpyridine) complexes
 possessing severe helical twists
;
_journal_issue                   11
_journal_name_full               'Chemical Communications'
_journal_page_first              1938
_journal_page_last               1940
_journal_paper_doi               10.1039/b921667g
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C46 H40 N2'
_chemical_formula_weight         620.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.7890(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4736(7)
_cell_length_b                   5.9821(3)
_cell_length_c                   24.7092(14)
_cell_measurement_reflns_used    5737
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.57
_cell_volume                     1811.17(17)
_computing_cell_refinement       'SMART version 5.6'
_computing_data_collection       'SMART version 5.6'
_computing_data_reduction        'SAINT version 5/6.0'
_computing_publication_material  'SHELXTL 6.1'
_computing_structure_refinement  'SHELXTL 6.1'
_computing_structure_solution    'SHELXTL 6.1'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Siemens P4 automated diffractometer'
_diffrn_measurement_method       'Smart 1K CCD detector'
_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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11727
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.74
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.974
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular fragment'
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.150
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0795
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0799P)^2^+0.2633P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1768
_reflns_number_gt                2850
_reflns_number_total             4067
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b921667gsup1.cif
_cod_data_source_block           bw4ccd
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7111565