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_1518970
_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         'C116 H132 N14 Ru2, 4(F6 P), 5.5(C5 H12 O)'
_chemical_formula_sum            'C143.5 H198 F24 N14 O5.5 P4 Ru2'
_chemical_formula_weight         2989.17
_chemical_name_common            Ru(tbp)2tpphzRu
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-02-27T16:39:01-00:00
_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                90
_cell_angle_beta                 106.727(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.8215(8)
_cell_length_b                   44.8370(12)
_cell_length_c                   19.8740(5)
_cell_measurement_reflns_used    6211
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.622
_cell_measurement_theta_min      3.752
_cell_volume                     16915.4(10)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
        (compiled Aug  2 2013,16:46:58)
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_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)
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_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      150(2)
_diffrn_detector_area_resol_mean 10.3385
_diffrn_measured_fraction_theta_full 0.863
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0237937
_diffrn_orient_matrix_UB_12      0.0309015
_diffrn_orient_matrix_UB_13      0.0182651
_diffrn_orient_matrix_UB_21      0.0127543
_diffrn_orient_matrix_UB_22      0.0129997
_diffrn_orient_matrix_UB_23      -0.0669941
_diffrn_orient_matrix_UB_31      -0.0766287
_diffrn_orient_matrix_UB_32      -0.007407
_diffrn_orient_matrix_UB_33      -0.0415685
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.863
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26007
_diffrn_reflns_point_group_measured_fraction_full 0.863
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.464
_diffrn_reflns_theta_min         7.48
_exptl_absorpt_coefficient_mu    2.45
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.91655
_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-orange
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_description       prism
_exptl_crystal_F_000             6260
_exptl_crystal_size_max          0.2754
_exptl_crystal_size_mid          0.1604
_exptl_crystal_size_min          0.1417
_platon_squeeze_details
;
;
_refine_diff_density_max         0.978
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         14622
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0658
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1423P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2178
_reflns_number_gt                10025
_reflns_number_total             14622
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00214a2.cif
_cod_data_source_block           Ru(tbp)2tpphzRu
_cod_depositor_comments
'Adding full bibliography for 1518963--1518971.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C143.50 H198 F24 N14 O5.50 P4 Ru2'
_cod_database_code               1518970