Water Oxidation Initiated by In Situ Dimerization of the Molecular Ru(pdc) Catalyst
Daniel, Quentin; Duan, Lele; Timmer, Brian J. J.; Chen, Hong; Luo, Xiaodan; Ambre, Ram; Wang, Ying; Zhang, Biaobiao; Zhang, Peili; Wang, Lei; Li, Fusheng; Sun, Junliang; Ahlquist, Mårten; Sun, Licheng; ACS Catalysis 8 (2018) 4375–; doi:10.1021/acscatal.7b03768

data_4515608
_publ_section_title
;
 Water Oxidation Initiated by In Situ Dimerization of the Molecular
 Ru(pdc) Catalyst
;
_journal_issue                   5
_journal_name_full               'ACS Catalysis'
_journal_page_first              4375
_journal_paper_doi               10.1021/acscatal.7b03768
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C34 H26 N6 O9 Ru2, F6 P'
_chemical_formula_sum            'C34 H26 F6 N6 O9 P Ru2'
_chemical_formula_weight         1009.72
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.201(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8587(8)
_cell_length_b                   23.8714(12)
_cell_length_c                   12.5805(9)
_cell_measurement_reflns_used    4418
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.8150
_cell_measurement_theta_min      1.9900
_cell_volume                     3765.8(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -36.54  21.76   1.10   30.00    --   -5.70  83.74-101.95   53
  2  \f     -9.68 350.02   1.10   30.00  73.80  -5.70  30.17    --   327
  3  \w    -36.54  21.76   1.10   30.00    --   -5.70  83.74  42.05   53
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0369262000
_diffrn_orient_matrix_UB_12      0.0224778000
_diffrn_orient_matrix_UB_13      0.0185278000
_diffrn_orient_matrix_UB_21      0.0088087000
_diffrn_orient_matrix_UB_22      -0.0031322000
_diffrn_orient_matrix_UB_23      -0.0512444000
_diffrn_orient_matrix_UB_31      -0.0419586000
_diffrn_orient_matrix_UB_32      0.0191644000
_diffrn_orient_matrix_UB_33      -0.0302130000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_unetI/netI     0.0561
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            59843
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.356
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.781
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.713
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6638
_refine_ls_number_restraints     552
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0992
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+31.2546P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4391
_reflns_number_total             6638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b03768_si_002.cif
_cod_data_source_block           p21c_a
_cod_database_code               4515608
_chemical_oxdiff_formula         Ru2C34H26F6N6O11P
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
 C30(H30), C31(H31), C32(H32)
;
_shelx_res_checksum              62335
_shelx_hkl_checksum              73935
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.837