Catalyst-solvent interactions in a dinuclear Ru-based water oxidation catalyst.
Shatskiy, Andrey; Lomoth, Reiner; Abdel-Magied, Ahmed F; Rabten, Wangchuk; Laine, Tanja M.; Chen, Hong; Sun, Junliang; Andersson, Pher G.; Kärkäs, Markus D; Johnston, Eric V.; Åkermark, Björn; Dalton transactions (Cambridge, England : 2003) 45 (2016) 19024–19033; doi:10.1039/c6dt03789e

data_7041155
_publ_section_title
;
 Catalyst-solvent interactions in a dinuclear Ru-based water oxidation
 catalyst.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              19024
_journal_page_last               19033
_journal_paper_doi               10.1039/c6dt03789e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C56 H52 N10 O6 Ru2, 2(C2 H3 N), 2(O)'
_chemical_formula_sum            'C60 H58 N12 O8 Ru2'
_chemical_formula_weight         1277.34
_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_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_date             2015-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-09-28 deposited with the CCDC.
2016-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.611(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7785(7)
_cell_length_b                   23.8622(11)
_cell_length_c                   23.4218(15)
_cell_measurement_reflns_used    7130
_cell_measurement_temperature    298
_cell_measurement_theta_max      26.7670
_cell_measurement_theta_min      3.3570
_cell_volume                     5921.0(6)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            39673
_diffrn_reflns_theta_full        26.0000
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.20
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
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    1.4328
_exptl_crystal_description       block
_exptl_crystal_F_000             2607.0924
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of CH3CN and water by slow evaporation'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.4115
_refine_diff_density_min         -0.9480
_refine_diff_density_rms         0.1747
_refine_ls_d_res_high            0.8400
_refine_ls_d_res_low             6.3608
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    100
_refine_ls_number_parameters     747
_refine_ls_number_reflns         10441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0130
_refine_ls_R_factor_all          0.0884
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.0488
_refine_ls_shift/su_mean         0.0006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0978P)^2^+4.5614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1740
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              28
_reflns_limit_k_min              0
_reflns_limit_l_max              27
_reflns_limit_l_min              0
_reflns_number_gt                7864
_reflns_number_total             10441
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt03789e2.cif
_cod_data_source_block           p21a_a
_cod_depositor_comments          'Adding full bibliography for 7041155.cif.'
_cod_database_code               7041155
_cell_oxdiff_length_a            10.7816(8)
_cell_oxdiff_length_b            23.8450(10)
_cell_oxdiff_length_c            23.4257(10)
_cell_oxdiff_angle_alpha         89.942(4)
_cell_oxdiff_angle_beta          100.526(5)
_cell_oxdiff_angle_gamma         90.056(5)
_cell_oxdiff_volume              5921.1(6)
_cell_oxdiff_measurement_reflns_used 7130
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
3. 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
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29),
  C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C38(H38), C39(H39),
 C41(H41), C42(H42), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50), C51(H51),
  C53(H53), C54(H54), C59(H59)
4.b Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C31(H31a,H31b,H31c), C37(H37a,H37b,H37c), C43(H43a,H43b,
 H43c), C49(H49a,H49b,H49c), C55(H55a,H55b,H55c), C57(H57a,H57b,H57c), C60(H60a,
 H60b,H60c)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a glass fibre with two-component glue'
_olex2_submission_special_instructions 'No special instructions were received'