Water oxidation by an electropolymerized catalyst on derivatized mesoporous metal oxide electrodes.
Ashford, Dennis L.; Lapides, Alexander M.; Vannucci, Aaron K.; Hanson, Kenneth; Torelli, Daniel A.; Harrison, Daniel P.; Templeton, Joseph L.; Meyer, Thomas J.; Journal of the American Chemical Society 136 (2014) 6578–6581; doi:10.1021/ja502464s

data_4121727
_publ_section_title
;
 Water oxidation by an electropolymerized catalyst on derivatized
 mesoporous metal oxide electrodes.
;
_journal_issue                   18
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6578
_journal_page_last               6581
_journal_paper_doi               10.1021/ja502464s
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety
'C37 H32 N8 Ru, 2(B F4), 2.5(H2 O), 2.5(C2 H3 N)'
_chemical_formula_sum            'C42 H44.5 B2 F8 N10.5 O2.5 Ru'
_chemical_formula_weight         1011.07
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-04-22
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Apr  9 2013 14:10:59, GUI svn.r4458)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.458(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0462(4)
_cell_length_b                   25.0845(6)
_cell_length_c                   19.0686(4)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      2.32
_cell_volume                     9101.9(3)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0799
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            66621
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.244
_diffrn_reflns_theta_min         2.322
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.511
_exptl_absorpt_correction_T_max  0.9089
_exptl_absorpt_correction_T_min  0.4874
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0806 before and 0.0627 after correction.
The Ratio of minimum to maximum transmission is 0.5363.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             4128
_exptl_crystal_size_max          0.461
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.042
_refine_diff_density_max         1.026
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1197
_refine_ls_number_reflns         16885
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0687
_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^)+(0.0909P)^2^+12.6794P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10761
_reflns_number_total             16885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja502464s_si_001.cif
_cod_data_source_block           x1304007
_cod_depositor_comments          'Adding full bibliography for 4121727.cif.'
_cod_database_code               4121727
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups, All O(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N18) \\sim Ueq, Uanis(C77) \\sim Ueq, Uanis(C78) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,O4,H4A,H4B), O3(H3B), O5(H5A,H5B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C18(H18), C19(H19), C20(H20), C21(H21), C26(H26), C27(H27), C28(H28), C33(H33),
  C34(H34), C35(H35), C36(H36), C38(H38), C40(H40), C41(H41), C44(H44),
 C45(H45), C47(H47), C48(H48), C50(H50), C55(H55), C56(H56), C57(H57), C58(H58),
  C63(H63), C64(H64), C65(H65), C70(H70), C71(H71), C72(H72), C73(H73)
3.c X=CH2 refined with riding coordinates:
 C12(H12A,H12B), C14(H14A,H14B), C49(H49A,H49B), C51(H51A,H51B)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C53(H53A,H53B,
 H53C), C60(H60A,H60B,H60C), C68(H68A,H68B,H68C), C76(H76A,H76B,H76C), C78(H78A,
 H78B,H78C), C80(H80A,H80B,H80C), C82(H82A,H82B,H82C), C84(H84A,H84B,H84C)
;
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.294
_shelx_hkl_checksum              58422
_shelx_res_checksum              81302
_shelxl_version_number           2013-2