Intramolecular proton transfer boosts water oxidation catalyzed by a Ru complex.
Matheu, Roc; Ertem, Mehmed Z.; Benet-Buchholz, Jordi; Coronado, Eugenio; Batista, Victor S.; Sala, Xavier; Llobet, Antoni; Journal of the American Chemical Society  (2015) 150812101708002–; doi:10.1021/jacs.5b06541

data_4124267
_publ_section_title
;
 Intramolecular proton transfer boosts water oxidation catalyzed by a Ru
 complex.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              150812101708002
_journal_paper_doi               10.1021/jacs.5b06541
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H24 N5 O5.5 Ru'
_chemical_formula_weight         619.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7358(7)
_cell_length_b                   28.7040(11)
_cell_length_c                   9.5921(4)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.42
_cell_measurement_theta_min      2.39
_cell_volume                     5158.6(4)
_computing_cell_refinement       'Bruker APEX2 v2011.4-0'
_computing_data_collection       'Bruker APEX2 v2011.4-0'
_computing_data_reduction        'Bruker SAINT V7.60A'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_detector_type            '4K CCD area detector APEX II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Kappa 4-axis goniometer bruker-nonius'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_measurement_specimen_support 'magnetic support with MicroMount'
_diffrn_radiation_monochromator  'Multilayer Montel 200 mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            41967
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.064
_diffrn_reflns_theta_min         1.787
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_current           70
_diffrn_source_power             50
_diffrn_source_size              '0.3 mm x 0.3 mm fine focus'
_diffrn_source_type              'Bruker-Nonius FR 591'
_exptl_absorpt_coefficient_mu    0.660
_exptl_absorpt_correction_T_max  0.9615
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
 SADABS Version 2008/1 Bruker-Nonius
 Blessing, Acta Cryst. (1995) A51 33-38
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             2520
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.205
_refine_diff_density_min         -1.036
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 5739 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.022(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         15870
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0406P)^2^+3.1186P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.0910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14569
_reflns_number_total             15870
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5b06541_si_002.cif
_cod_data_source_block           Roc_tda1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)2(1)2
_cod_original_formula_sum        'C28 H24 N5 O5.50 Ru'
_cod_database_code               4124267
_shelx_estimated_absorpt_t_min   0.852
_shelx_estimated_absorpt_t_max   0.961
_shelxl_version_number           2012-9
_shelx_res_checksum              49863
_shelx_hkl_checksum              42789