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_1544713
_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 Cl Os, P1 F6'
_chemical_formula_sum            'C29 H25 Cl F6 N5 Os P'
_chemical_formula_weight         814.16
_chemical_name_systematic
;
OsPY5Me2Cl_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             2015-10-01T13:44:10-00:00
_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                   8.978(2)
_cell_length_b                   17.366(5)
_cell_length_c                   20.947(6)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.14
_cell_measurement_wavelength     0.71073
_cell_volume                     3265.9(15)
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_type       d*trek
_diffrn_orient_matrix_UB_11      0.1114
_diffrn_orient_matrix_UB_12      -0.0024
_diffrn_orient_matrix_UB_13      0.001
_diffrn_orient_matrix_UB_21      0.0013
_diffrn_orient_matrix_UB_22      0.0468
_diffrn_orient_matrix_UB_23      -0.0335
_diffrn_orient_matrix_UB_31      0.0002
_diffrn_orient_matrix_UB_32      0.0278
_diffrn_orient_matrix_UB_33      0.0388
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22873
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         3.211
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
TITL SIR97 run in space group P b c m
CELL    8.9780   17.3660   20.9470     90.00     90.00     90.00
SPGR Pbcm
C101 0.500 0.500 0.500 !       3.60 eA-3
C102 0.418 0.570 0.076 !       2.83 eA-3
C103 0.534 0.543 0.458 !       2.06 eA-3
C104 0.432 0.517 0.461 !       1.73 eA-3
C105 0.592 0.040 0.028 !       1.69 eA-3
Q106 0.713 0.250 0.249 !       1.40 eA-3
Q107 0.132 0.422 0.247 !       1.12 eA-3
Q108 0.137 0.312 0.246 !       0.98 eA-3
Q109 0.879 0.031 0.251 !       0.61 eA-3
Q110 0.496 0.876 0.189 !       0.54 eA-3
Q111 0.313 0.922 0.249 !       0.53 eA-3
Q112 0.029 0.250 0.000 !       0.53 eA-3
Q113 0.313 0.375 0.248 !       0.53 eA-3
Q114 0.383 0.374 0.207 !       0.51 eA-3
;
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     215
_refine_ls_number_reflns         3801
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.019
_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^)+(0.0276P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0485
_refine_ls_wR_factor_ref         0.0493
_reflns_Friedel_coverage         0
_reflns_number_gt                3371
_reflns_number_total             3801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6fd00227g2.cif
_cod_data_source_block           OsPY5Me2Cl_PF6
_cod_original_formula_sum        'C29 H25 Cl1 F6 N5 Os1 P1'
_cod_database_code               1544713
_shelx_estimated_absorpt_t_min   0.404
_shelx_estimated_absorpt_t_max   0.709
_platon_squeeze_void_probe_radius 1.20