Triphenylphosphine Photorelease and Induction of Catalytic Activity from Ruthenium-Arene Complexes Bearing a Photoswitchable o-Tosylamide Azobenzene Ligand
Deo, Claire; Bogliotti, Nicolas; Retailleau, Pascal; Xie, Juan; Organometallics 35 (2016) 2694–; doi:10.1021/acs.organomet.6b00431

data_4088785
_publ_section_title
;
 Triphenylphosphine Photorelease and Induction of Catalytic Activity from
 Ruthenium-Arene Complexes Bearing a Photoswitchable o-Tosylamide
 Azobenzene Ligand
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              2694
_journal_paper_doi               10.1021/acs.organomet.6b00431
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         ' C49 H49 N3 O2 P Ru S, F6 P, C H2 Cl2'
_chemical_formula_sum            'C50 H51 Cl2 F6 N3 O2 P2 Ru S'
_chemical_formula_weight         1105.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                96.783(3)
_cell_angle_beta                 101.973(3)
_cell_angle_gamma                106.259(3)
_cell_formula_units_Z            2
_cell_length_a                   10.4176(7)
_cell_length_b                   12.9740(9)
_cell_length_c                   19.5787(14)
_cell_measurement_reflns_used    586
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.1
_cell_volume                     2441.0(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXLT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36250
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         3.231
_diffrn_source                   'Rigaku microsource mm003'
_exptl_absorpt_coefficient_mu    0.605
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       cobbledstone
_exptl_crystal_F_000             1132
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.902
_refine_diff_density_min         -0.859
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         8840
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0871
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0886P)^2^+8.6438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1878
_refine_ls_wR_factor_ref         0.2008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7414
_reflns_number_total             8881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00431_si_001.cif
_cod_data_source_block           Z3
_cod_database_code               4088785
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              92878
_shelx_hkl_checksum              30902