Second Coordination Sphere Effects in an Evolved Ru Complex Based on a Highly Adaptable Ligand Results in Rapid Water Oxidation Catalysis.
Vereshchuk, Nataliia; Matheu, Roc; Benet-Buchholz, Jordi; Pipelier, Muriel; Lebreton, Jacques; Dubreuil, Didier; Tessier, Arnaud; Gimbert-Suriñach, Carolina; Ertem, Mehmed Z.; Llobet, Antoni; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.9b11935

data_4134335
_publ_section_title
;
 Second Coordination Sphere Effects in an Evolved Ru Complex Based on a
 Highly Adaptable Ligand Results in Rapid Water Oxidation Catalysis.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11935
_journal_year                    2020
_chemical_formula_sum            'C26 H39 Cs3 N5 O16.5 P2 Ru'
_chemical_formula_weight         1247.36
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                63.2183(12)
_cell_angle_beta                 67.7101(15)
_cell_angle_gamma                71.5300(14)
_cell_formula_units_Z            4
_cell_length_a                   15.8725(10)
_cell_length_b                   17.0940(10)
_cell_length_c                   17.9384(11)
_cell_measurement_reflns_used    9798
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.53
_cell_measurement_theta_min      2.22
_cell_volume                     3957.1(4)
_computing_cell_refinement       'Bruker APEX3 v2015.9-0'
_computing_data_collection       'Bruker APEX3 v2015.9-0'
_computing_data_reduction        'Bruker SAINT V8.35A'
_computing_molecular_graphics
;
 SHELXle: C.B. Huebschle, G.M. Sheldrick & B. Dittrich
 J.Appl.Cryst. (2011) 44, 1281-1284.
;
_computing_publication_material  'XCIF, SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT V2014/4 (Sheldrick 2014)'
_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 0.991
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'APEX DUO Kappa 4-axis goniometer'
_diffrn_measurement_method
;
 Fullsphere data collection, phi and omega scans
;
_diffrn_radiation_monochromator  'Quazar MX Multilayer Optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0537
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            76682
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.876
_diffrn_reflns_theta_min         1.583
_diffrn_source                   'Microfocus source E025 IuS'
_diffrn_source_current           0.6
_diffrn_source_power             50
_diffrn_source_size              '0.2 mm x 0.2 mm fine focus'
_diffrn_source_type              'Bruker APEX DUO'
_exptl_absorpt_coefficient_mu    3.271
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.5772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2014/4
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.094
_exptl_crystal_description       block
_exptl_crystal_F_000             2404
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.039
_refine_diff_density_min         -3.118
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1128
_refine_ls_number_reflns         30243
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0371P)^2^+15.1346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1053
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23470
_reflns_number_total             30243
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11935_si_002.cif
_cod_data_source_block           mo_TPAaqua_0m
_cod_original_formula_sum        'C26 H39 Cs3 N5 O16.50 P2 Ru'
_cod_database_code               4134335
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.561
_shelx_estimated_absorpt_t_max   0.937
_shelx_res_checksum              63588
_shelx_hkl_checksum              62977