1,10-Phenanthroline-dithiine iridium and ruthenium complexes: synthesis, characterization and photocatalytic dihydrogen evolution.
Erdmann, E.; Villinger, A.; König, B; Seidel, W. W.; Photochemical & photobiological sciences : Official journal of the European Photochemistry Association and the European Society for Photobiology 17 (2018) 1056–1067; doi:10.1039/c8pp00068a

data_1549500
_publ_section_title
;
 1,10-Phenanthroline-dithiine iridium and ruthenium complexes: synthesis,
 characterization and photocatalytic dihydrogen evolution.
;
_journal_issue                   8
_journal_name_full
'Photochemical &amp; photobiological sciences : Official journal of the European Photochemistry Association and the European Society for Photobiology'
_journal_page_first              1056
_journal_page_last               1067
_journal_paper_doi               10.1039/c8pp00068a
_journal_volume                  17
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C42 H26 Ir N6 S2 +, F6 P  -, 0.5 (C H2 Cl2)'
_chemical_formula_sum            'C42.5 H27 Cl F6 Ir N6 P S2'
_chemical_formula_weight         1058.44
_chemical_name_systematic
1,10-phenanthrolinedithiino[2,3-b]quinoxaline-bis(phendiylpyridine)iridium(III)-hexafluorophosphate
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-02-13 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.785(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.4564(8)
_cell_length_b                   13.5405(5)
_cell_length_c                   25.1871(9)
_cell_measurement_reflns_used    9438
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.05
_cell_measurement_theta_min      2.21
_cell_volume                     7654.9(5)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0593
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            117421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         0.809
_exptl_absorpt_coefficient_mu    3.782
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.4786
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       block
_exptl_crystal_F_000             4152
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane'
_exptl_crystal_size_max          0.599
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.156
_refine_diff_density_max         2.224
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.458(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2114
_refine_ls_number_reflns         39954
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0469P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1116
_reflns_Friedel_coverage         0.924
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                26368
_reflns_number_total             39954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8pp00068a2.cif
_cod_data_source_block           ah_ee66
_cod_depositor_comments
'Adding full bibliography for 1549499--1549500.cif.'
_cod_original_formula_sum        'C42.50 H27 Cl F6 Ir N6 P S2'
_cod_database_code               1549500
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.210
_shelx_estimated_absorpt_t_max   0.590
_shelx_res_checksum              96555