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_1544714
_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 H27 N5 O1 Fe, 2(P1 F6)'
_chemical_formula_sum            'C29 H33 F12 Fe N5 O4 P2'
_chemical_formula_weight         861.39
_chemical_name_systematic
;
FePY5Me2OH2_PF6
;
_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             2015-10-01T14:38:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-10-07 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;
_cell_angle_alpha                72.8880(10)
_cell_angle_beta                 65.5780(10)
_cell_angle_gamma                66.9360(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6708(3)
_cell_length_b                   12.9661(3)
_cell_length_c                   13.4037(4)
_cell_measurement_reflns_used    15259
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.03
_cell_measurement_wavelength     0.71073
_cell_volume                     1677.90(8)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction
'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector                 'curved image-plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_UB_11      0.08406
_diffrn_orient_matrix_UB_12      -0.041805
_diffrn_orient_matrix_UB_13      -0.053434
_diffrn_orient_matrix_UB_21      0.051678
_diffrn_orient_matrix_UB_22      0.028037
_diffrn_orient_matrix_UB_23      0.023975
_diffrn_orient_matrix_UB_31      0.007946
_diffrn_orient_matrix_UB_32      -0.068355
_diffrn_orient_matrix_UB_33      0.058783
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16616
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_min         3.037
_diffrn_source                   'rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1955)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     640
_refine_ls_number_reflns         7611
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0695P)^2^+0.3549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1053
_refine_ls_wR_factor_ref         0.1083
_reflns_Friedel_coverage         0
_reflns_number_gt                6804
_reflns_number_total             7611
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00227g2.cif
_cod_data_source_block           FePY5Me2OH2_PF6
_cod_database_code               1544714
_shelx_estimated_absorpt_t_min   0.937
_shelx_estimated_absorpt_t_max   0.937