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_4130713
_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 Cl4 N5 O7 Ru2, 2(C H2 Cl2)'
_chemical_formula_sum            'C22 H16 Cl8 N5 O7 Ru2'
_chemical_formula_weight         948.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90.050(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.2028(13)
_cell_length_b                   15.4349(11)
_cell_length_c                   11.5463(8)
_cell_measurement_reflns_used    9273
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.4969
_cell_measurement_theta_min      2.5000
_cell_volume                     3065.8(4)
_computing_cell_refinement       'SAINT+ Ver. 7.68A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 Ver. 2014.11-0 (Bruker-AXS, 2014)'
_computing_data_reduction        'SAINT+ Ver. 8.34A (Bruker-AXS, 2014)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008-2012)'
_diffrn_ambient_temperature      100.0
_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 0.993
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_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_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            83507
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.533
_diffrn_reflns_theta_min         1.184
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  0.7057
_exptl_absorpt_correction_T_min  0.3649
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.728
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.216
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.542
_refine_diff_density_rms         0.093
_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_parameters     409
_refine_ls_number_reflns         9327
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.292
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0294P)^2^+4.3328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9075
_reflns_number_total             9327
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b05942_si_002.cif
_cod_data_source_block           compound4
_cod_database_code               4130713
_shelx_estimated_absorpt_t_max   0.706
_shelx_estimated_absorpt_t_min   0.365
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5351(6) 0.4649(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
3. Restrained distances
 Cl5-C21 \\sim C21-C21 \\sim Cl8-C22 \\sim Cl8A-C22 \\sim Cl7-C22
 with sigma of 0.005
 Cl6A-C21A \\sim Cl6-C21 \\sim Cl5-C21 \\sim Cl5-C21A \\sim Cl8-C22 \\sim
Cl8A-C22 \\sim Cl7-C22
 with sigma of 0.005
4. Uiso/Uaniso restraints and constraints
Uanis(Cl8) = Uanis(Cl8A)
Uanis(Cl6A) = Uanis(Cl6)
Uanis(C21) = Uanis(C21A)
5. Others
 Sof(Cl8A)=Sof(H22C)=Sof(H22D)=1-FVAR(1)
 Sof(Cl8)=Sof(H22A)=Sof(H22B)=FVAR(1)
 Sof(Cl6A)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(2)
 Sof(Cl6)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C21A(H21C,H21D), C22(H22A,H22B), C22(H22C,H22D)
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              64383
_shelx_hkl_checksum              25394
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'