Rapid water oxidation electrocatalysis by a ruthenium complex of the tripodal ligand tris(2-pyridyl)phosphine oxide
Walden, Andrew G.; Miller, Alexander J. M.; Chem. Sci. 6 (2015) 2405–; doi:10.1039/C5SC00032G

data_1518672
_publ_section_title
;
 Rapid water oxidation electrocatalysis by a ruthenium complex of the
 tripodal ligand tris(2-pyridyl)phosphine oxide
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2405
_journal_paper_doi               10.1039/C5SC00032G
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C25 H20 Cl N5 O P Ru, F6 P, 2(C H2 Cl2)'
_chemical_formula_sum            'C27 H24 Cl5 F6 N5 O P2 Ru'
_chemical_formula_weight         888.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-11-17
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4709)
;
_audit_update_record
;
2014-11-17 deposited with the CCDC.
2015-02-04 downloaded from the CCDC.
;
_cell_angle_alpha                67.197(6)
_cell_angle_beta                 84.942(6)
_cell_angle_gamma                67.025(6)
_cell_formula_units_Z            2
_cell_length_a                   11.14450(10)
_cell_length_b                   12.05480(10)
_cell_length_c                   14.8726(2)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      3.23
_cell_volume                     1691.09(12)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20592
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.063
_diffrn_reflns_theta_min         3.232
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.877
_exptl_absorpt_correction_T_max  0.4375
_exptl_absorpt_correction_T_min  0.2512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0797 before and 0.0504 after correction.
The Ratio of minimum to maximum transmission is 0.5742.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_description       Block
_exptl_crystal_F_000             884
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: '
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.193
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         6160
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0417P)^2^+3.4718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5391
_reflns_number_total             6160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc00032g2.cif
_cod_data_source_block           p1bar_a
_cod_depositor_comments          'Adding full bibliography for 1518672.cif.'
_cod_original_cell_volume        1691.09(10)
_cod_database_code               1518672
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.370
_shelx_estimated_absorpt_t_min   0.212
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Cl6 \\sim C28 \\sim Cl5 \\sim C27 \\sim Cl4: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Others
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(Cl4)=1-FVAR(1)
 Sof(Cl6)=Sof(C28)=Sof(H28A)=Sof(H28B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C6(H6), C2(H2), C25(H25), C22(H22), C19(H19), C14(H14), C24(H24),
 C12(H12), C9(H9), C17(H17), C4(H4), C18(H18), C7(H7), C23(H23), C16(H16),
 C8(H8), C13(H13), C3(H3), C1(H1)
;
_shelx_res_checksum              99563