A Synthetic Oxygen Atom Transfer Photocycle from a Diruthenium Oxyanion Complex.
Corcos, Amanda R.; Pap, József S; Yang, Tzuhsiung; Berry, John F.; Journal of the American Chemical Society 138 (2016) 10032–10040; doi:10.1021/jacs.6b05942

data_4130714
_publ_section_title
;
 A Synthetic Oxygen Atom Transfer Photocycle from a Diruthenium Oxyanion
 Complex.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10032
_journal_page_last               10040
_journal_paper_doi               10.1021/jacs.6b05942
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C20 H12 Cl5 N4 O8 Ru2, 2(C H2 Cl2)'
_chemical_formula_sum            'C22 H16 Cl9 N4 O8 Ru2'
_chemical_formula_weight         985.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 93.965(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5392(6)
_cell_length_b                   16.7038(9)
_cell_length_c                   16.6387(9)
_cell_measurement_reflns_used    5105
_cell_measurement_temperature    100.1
_cell_measurement_theta_max      26.360
_cell_measurement_theta_min      2.413
_cell_volume                     3199.4(3)
_computing_data_collection       'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2015b)'
_computing_structure_solution    'XT (Sheldrick, 2015a)'
_diffrn_ambient_temperature      100.1
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6580
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.415
_diffrn_reflns_theta_min         1.730
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.745372
_exptl_absorpt_correction_T_min  0.614358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1513 before and 0.0575 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1653 before and 0.0604 after correction.
 The Ratio of minimum to maximum transmission is 0.83.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 111351 reflections, Rint = 0.0660
 (45816 with I > 3sig(I), Rint = 0.0499)
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1924
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.094
_refine_diff_density_max         1.215
_refine_diff_density_min         -0.684
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         6580
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0473
_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^)+(0.0310P)^2^+16.7071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5531
_reflns_number_total             6580
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05942_si_002.cif
_cod_data_source_block           compound5
_cod_database_code               4130714
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.760
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5974(11) 0.4026(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 Cl9A-C22A = Cl9-C22 = Cl8-C22 = Cl8A-C22A = Cl7A-C21A = Cl6A-C21A = Cl7-C21 =
 Cl6-C21
 1.73922 with sigma of 0.01
 Cl6-Cl7 = Cl6A-Cl7A = Cl8-Cl9 = Cl8A-Cl9A
 2.89928 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Cl8A \\sim Cl9A \\sim C22A \\sim Cl8 \\sim Cl9 \\sim C22: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Cl6 \\sim Cl7 \\sim C21 \\sim Cl6A \\sim Cl7A \\sim C21A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(Ru1) = Uanis(Ru1A)
5. Others
 Sof(Cl8A)=Sof(Cl9A)=Sof(C22A)=Sof(H22A)=Sof(H22B)=1-FVAR(1)
 Sof(Cl8)=Sof(Cl9)=Sof(C22)=Sof(H22C)=Sof(H22D)=FVAR(1)
 Sof(Cl6A)=Sof(Cl7A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(2)
 Sof(Cl6)=Sof(Cl7)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(2)
 1(DFIX)=FVAR(3)
 1(DFIX)=1.667*FVAR(4)
 Sof(Ru1A)=1-FVAR(4)
 Sof(Ru1)=FVAR(4)
6.a Secondary CH2 refined with riding coordinates:
 C22A(H22A,H22B), C22(H22C,H22D), C21(H21A,H21B), C21A(H21C,H21D)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19)
;
_shelx_res_checksum              47769
_shelx_hkl_checksum              63055
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'