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_1549499
_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_formula_moiety
;
C34 H22 Br2 Ir N4 +, F6 P -, C H2 Cl2, C2 H3 N
;
_chemical_formula_sum            'C37 H27 Br2 Cl2 F6 Ir N5 P'
_chemical_formula_weight         1109.52
_chemical_name_systematic
5,6-Dibromido-1,10-phenanthroline-bis(phendiylpyridine)iridium(III)-hexafluorophosphate
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-02-13 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.389(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2183(10)
_cell_length_b                   13.7802(9)
_cell_length_c                   19.1871(12)
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.68
_cell_measurement_theta_min      2.60
_cell_volume                     3728.1(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.983
_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  0.0635
_diffrn_reflns_av_unetI/netI     0.1093
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42814
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.993
_diffrn_reflns_theta_min         2.066
_exptl_absorpt_coefficient_mu    5.978
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.977
_exptl_crystal_description       block
_exptl_crystal_F_000             2136
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, acetonitrile'
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.100
_platon_squeeze_details
;
The unit cell contains four dichloromethane and four acetonitrile molecules 
which have been treated as a diffuse contribution to the overall scattering 
without specific atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         2.452
_refine_diff_density_min         -1.855
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         9740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0632P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1218
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5929
_reflns_number_total             9740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8pp00068a2.cif
_cod_data_source_block           is_tae034
_cod_depositor_comments
'Adding full bibliography for 1549499--1549500.cif.'
_cod_database_code               1549499
_shelx_estimated_absorpt_t_min   0.276
_shelx_estimated_absorpt_t_max   0.586
_shelx_res_checksum              45018