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_4088786
_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         'C43 H61 N3 O2 P Ru S, F6 P'
_chemical_formula_sum            'C43 H61 F6 N3 O2 P2 Ru S'
_chemical_formula_weight         961.01
_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                81.341(4)
_cell_angle_beta                 85.254(4)
_cell_angle_gamma                74.297(4)
_cell_formula_units_Z            2
_cell_length_a                   10.2681(7)
_cell_length_b                   14.6075(10)
_cell_length_c                   15.5975(11)
_cell_measurement_reflns_used    958
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.4
_cell_volume                     2224.3(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    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
	Number of images: 252
	           Slice: -91.0000 - 35.0000
	     Image width: 0.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -8.0000
	             Phi: 0.0000
	             XTD: 30.0000
	          2theta: -1.0000
scan:
	Number of images: 248
	           Slice: -91.0000 - 33.0000
	     Image width: 0.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: 0.0000
	             XTD: 30.0000
	          2theta: -1.0000
scan:
	Number of images: 194
	           Slice: -64.0000 - 33.0000
	     Image width: 0.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -144.0000
	             XTD: 30.0000
	          2theta: -1.0000
scan:
	Number of images: 128
	           Slice: -53.0000 - 11.0000
	     Image width: 0.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: -72.0000
	             XTD: 30.0000
	          2theta: -1.0000
scan:
	Number of images: 95
	           Slice: -66.5000 - -19.0000
	     Image width: 0.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: -72.0000
	             Phi: 72.0000
	             XTD: 30.0000
	          2theta: -1.0000
scan:
	Number of images: 90
	           Slice: -4.0000 - 41.0000
	     Image width: 0.5000
	        Exp time: 60.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	           Kappa: 40.0000
	             Phi: -108.0000
	             XTD: 30.0000
	          2theta: -1.0000

;
_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_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.030944
_diffrn_orient_matrix_UB_12      -0.078465
_diffrn_orient_matrix_UB_13      0.056032
_diffrn_orient_matrix_UB_21      -0.005368
_diffrn_orient_matrix_UB_22      -0.025571
_diffrn_orient_matrix_UB_23      -0.066828
_diffrn_orient_matrix_UB_31      0.060116
_diffrn_orient_matrix_UB_32      0.024037
_diffrn_orient_matrix_UB_33      -0.004715
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1249
_diffrn_reflns_av_unetI/netI     0.0768
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37485
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.348
_diffrn_reflns_theta_min         3.651
_diffrn_reflns_transf_matrix_11  0.030944
_diffrn_reflns_transf_matrix_12  -0.078465
_diffrn_reflns_transf_matrix_13  0.056032
_diffrn_reflns_transf_matrix_21  -0.005368
_diffrn_reflns_transf_matrix_22  -0.025571
_diffrn_reflns_transf_matrix_23  -0.066828
_diffrn_reflns_transf_matrix_31  0.060116
_diffrn_reflns_transf_matrix_32  0.024037
_diffrn_reflns_transf_matrix_33  -0.004715
_diffrn_source                   MicroMax003_Mo
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB, (Higashi,1998)'
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.517
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         8107
_refine_ls_number_restraints     312
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1307
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5557
_reflns_number_total             8109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00431_si_001.cif
_cod_data_source_block           Z5
_cod_database_code               4088786
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              57485
_shelx_hkl_checksum              27616