Fe, Ru, and Os Complexes with the Same Molecular Framework: Comparison of Structures, Properties and Catalytic Activities
Yoshida, Masaki; Kondo, Mio; Okamura, Masaya; Kanaike, Mari; Haesuwannakij, Setsiri; Sakurai, Hidehiro; Masaoka, Shigeyuki; Faraday Discuss.  (2016) –; doi:10.1039/C6FD00227G

data_1544712
_publ_section_title
;
 Fe, Ru, and Os Complexes with the Same Molecular Framework: Comparison of
 Structures, Properties and Catalytic Activities
;
_journal_name_full               'Faraday Discuss.'
_journal_paper_doi               10.1039/C6FD00227G
_journal_year                    2016
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C29 H25 N5 Cl1 Ru1, P1 F6'
_chemical_formula_sum            'C29 H25 Cl F6 N5 P Ru'
_chemical_formula_weight         725.03
_chemical_name_systematic
;
RuPY5Me2Cl_PF6
;
_space_group_IT_number           57
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      57
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_space_group_name_H-M   'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-01T11:27:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-02-04 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9368(13)
_cell_length_b                   17.315(3)
_cell_length_c                   20.910(3)
_cell_measurement_reflns_used    8835
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.22
_cell_measurement_wavelength     0.71073
_cell_volume                     3235.6(9)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR-97 (Altomare et al, 1999)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.57
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       d*trek
_diffrn_orient_matrix_UB_11      -0.0338
_diffrn_orient_matrix_UB_12      0.077
_diffrn_orient_matrix_UB_13      0.0738
_diffrn_orient_matrix_UB_21      0.055
_diffrn_orient_matrix_UB_22      0.0142
_diffrn_orient_matrix_UB_23      0.0104
_diffrn_orient_matrix_UB_31      -0.0018
_diffrn_orient_matrix_UB_32      0.0327
_diffrn_orient_matrix_UB_33      -0.0349
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23789
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         3.221
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
TITL SIR97 run in space group P b c m
CELL    8.9368   17.3150   20.9100     90.00     90.00     90.00
SPGR Pbcm
C101 0.500 1.000 0.500 !       4.35 eA-3
C102 0.582 0.084 0.421 !       3.22 eA-3
Q103 0.131 0.312 0.244 !       2.56 eA-3
C104 0.530 0.547 0.458 !       2.37 eA-3
C105 0.596 0.039 0.034 !       1.91 eA-3
Q106 0.042 0.250 0.000 !       1.72 eA-3
Q107 0.714 0.250 0.249 !       1.09 eA-3
Q108 0.869 0.031 0.249 !       0.89 eA-3
Q109 0.945 0.745 0.084 !       0.71 eA-3
Q110 0.154 0.472 0.312 !       0.67 eA-3
Q111 0.866 0.359 0.251 !       0.67 eA-3
Q112 0.873 0.922 0.249 !       0.65 eA-3
Q113 0.345 0.922 0.250 !       0.64 eA-3
Q114 0.381 0.796 0.406 !       0.62 eA-3
Q115 0.552 0.797 0.255 !       0.61 eA-3
Q116 0.114 0.548 0.189 !       0.61 eA-3
Q117 0.434 0.353 0.193 !       0.60 eA-3
Q118 0.726 0.797 0.254 !       0.59 eA-3
Q119 0.168 0.188 0.500 !       0.59 eA-3
Q120 0.191 0.594 0.245 !       0.59 eA-3
Q121 0.419 0.869 0.314 !       0.58 eA-3
Q122 0.558 0.016 0.244 !       0.57 eA-3
Q123 0.590 0.656 0.244 !       0.55 eA-3
Q124 0.444 0.656 0.246 !       0.54 eA-3
Q125 0.507 0.781 0.098 !       0.54 eA-3
Q126 0.318 0.847 0.139 !       0.53 eA-3
Q127 0.915 0.316 0.504 !       0.50 eA-3
;
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3796
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0366P)^2^+2.0785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0735
_reflns_Friedel_coverage         0
_reflns_number_gt                3426
_reflns_number_total             3796
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00227g2.cif
_cod_data_source_block           RuPY5Me2Cl_PF6
_cod_original_formula_sum        'C29 H25 Cl1 F6 N5 P1 Ru1'
_cod_database_code               1544712
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.96
_platon_squeeze_void_probe_radius 1.20