Optimized synthesis of a tert-butyl-phenyl-substituted tetrapyridophenazine ligand and its Ru(ii) complexes and determination of dimerization behaviour of the complexes through supramolecular "Fingerhakel".
Ritter, K.; Pehlken, C.; Sorsche, D.; Rau, S.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 8889–8905; doi:10.1039/c5dt00214a

data_1518971
_publ_section_title
;
 Optimized synthesis of a tert-butyl-phenyl-substituted
 tetrapyridophenazine ligand and its Ru(ii) complexes and determination of
 dimerization behaviour of the complexes through supramolecular
 &quot;Fingerhakel&quot;.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8889
_journal_page_last               8905
_journal_paper_doi               10.1039/c5dt00214a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C68 H80 N6 Ru, 2(F6 P),3.5(C2 H3 N)'
_chemical_formula_sum            'C75 H90.5 F12 N9.5 P2 Ru'
_chemical_formula_weight         1516.07
_chemical_name_common            Ru(tbp)2phen
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-02-27T17:24:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-02-27 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                104.461(2)
_cell_angle_beta                 116.670(3)
_cell_angle_gamma                92.680(2)
_cell_formula_units_Z            2
_cell_length_a                   15.7991(4)
_cell_length_b                   16.8342(4)
_cell_length_c                   16.8521(5)
_cell_measurement_reflns_used    19703
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      76.323
_cell_measurement_theta_min      3.221
_cell_volume                     3812.4(2)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.3385
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0458088
_diffrn_orient_matrix_UB_12      -0.0581095
_diffrn_orient_matrix_UB_13      -0.1009691
_diffrn_orient_matrix_UB_21      -0.0398621
_diffrn_orient_matrix_UB_22      -0.0673606
_diffrn_orient_matrix_UB_23      0.0280393
_diffrn_orient_matrix_UB_31      -0.0929233
_diffrn_orient_matrix_UB_32      0.0364661
_diffrn_orient_matrix_UB_33      -0.0233163
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42405
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.493
_diffrn_reflns_theta_min         7.407
_exptl_absorpt_coefficient_mu    2.711
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1578
_exptl_crystal_size_max          0.2341
_exptl_crystal_size_mid          0.1185
_exptl_crystal_size_min          0.0612
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.07
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     979
_refine_ls_number_reflns         15533
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+3.1518P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.12
_reflns_number_gt                13862
_reflns_number_total             15533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00214a2.cif
_cod_data_source_block           Ru(tbp)2phen
_cod_depositor_comments
'Adding full bibliography for 1518963--1518971.cif.'
_cod_original_formula_sum        'C75 H90.50 F12 N9.50 P2 Ru'
_cod_database_code               1518971