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_1544711
_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 Cl Fe N5, F6 P'
_chemical_formula_sum            'C29 H25 Cl F6 Fe N5 P'
_chemical_formula_weight         679.81
_chemical_name_systematic
;
FePY5Me2Cl_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_creation_date             2015-09-30T17:23:40-00:00
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9422(3)
_cell_length_b                   17.1851(6)
_cell_length_c                   20.8463(8)
_cell_measurement_reflns_used    15905
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3
_cell_measurement_wavelength     0.71073
_cell_volume                     3203.5(2)
_computing_cell_refinement       'RAPID AUTO (Rigaku)'
_computing_data_collection       'RAPID AUTO (Rigaku)'
_computing_data_reduction        'RAPID AUTO (Rigaku)'
_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                 'curved image-plate'
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'quarter \C-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_UB_11      0.028306
_diffrn_orient_matrix_UB_12      0.029269
_diffrn_orient_matrix_UB_13      -0.039642
_diffrn_orient_matrix_UB_21      -0.092986
_diffrn_orient_matrix_UB_22      -0.018826
_diffrn_orient_matrix_UB_23      -0.021664
_diffrn_orient_matrix_UB_31      -0.055301
_diffrn_orient_matrix_UB_32      0.046636
_diffrn_orient_matrix_UB_33      0.016135
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29640
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.418
_diffrn_reflns_theta_min         3.001
_diffrn_source                   'rotating anode'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1955)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.41
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
TITL SIR97 run in space group P b c m
CELL    8.9422   17.1851   20.8463     90.00     90.00     90.00
SPGR Pbcm
C101 1.000 1.000 0.000 !       4.52 eA-3
C102 0.920 0.582 0.421 !       2.87 eA-3
C103 0.030 0.545 0.049 !       2.17 eA-3
C104 0.100 0.038 0.033 !       1.84 eA-3
Q105 0.935 0.406 0.252 !       1.05 eA-3
Q106 0.780 0.313 0.249 !       0.98 eA-3
Q107 0.218 0.874 0.316 !       0.84 eA-3
Q108 0.646 0.422 0.248 !       0.79 eA-3
Q109 0.278 0.855 0.281 !       0.77 eA-3
Q110 0.276 0.422 0.249 !       0.75 eA-3
Q111 0.664 0.470 0.263 !       0.64 eA-3
Q112 0.209 0.578 0.249 !       0.61 eA-3
Q113 0.646 0.516 0.254 !       0.61 eA-3
Q114 0.212 0.951 0.191 !       0.61 eA-3
Q115 0.946 0.906 0.253 !       0.60 eA-3
C116 0.096 1.001 0.396 !       0.59 eA-3
Q117 0.250 0.937 0.245 !       0.57 eA-3
Q118 0.664 0.297 0.500 !       0.55 eA-3
Q119 0.441 0.874 0.233 !       0.55 eA-3
Q120 0.472 0.906 0.249 !       0.53 eA-3
Q121 0.491 0.766 0.251 !       0.53 eA-3
Q122 0.143 0.858 0.258 !       0.52 eA-3
Q123 0.154 0.981 0.213 !       0.52 eA-3
Q124 0.383 0.250 0.500 !       0.51 eA-3
;
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.11
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0989P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1904
_reflns_Friedel_coverage         0
_reflns_number_gt                2261
_reflns_number_total             3741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00227g2.cif
_cod_data_source_block           FePY5Me2Cl_PF6
_cod_original_formula_sum        'C29 H25 Cl1 F6 Fe1 N5 P1'
_cod_database_code               1544711
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.936
_platon_squeeze_void_probe_radius 1.20