Characterization of a trinuclear ruthenium species in catalytic water oxidation by Ru(bda)(pic)2 in neutral media.
Zhang, Biaobiao; Li, Fei; Zhang, Rong; Ma, Chengbing; Chen, Lin; Sun, Licheng; Chemical communications (Cambridge, England) 52 (2016) 8619–8622; doi:10.1039/c6cc04003a

data_7124706
_publ_section_title
;
 Characterization of a trinuclear ruthenium species in catalytic water
 oxidation by Ru(bda)(pic)2 in neutral media.
;
_journal_issue                   55
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8619
_journal_page_last               8622
_journal_paper_doi               10.1039/c6cc04003a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C62 H59 N11 O11 Ru3, 2(F6 P)'
_chemical_formula_sum            'C62 H59 F12 N11 O11 P2 Ru3'
_chemical_formula_weight         1727.35
_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_date             2015-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2014.12.26 svn.r3119 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-24 deposited with the CCDC.
2016-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                107.027(4)
_cell_angle_beta                 102.696(3)
_cell_angle_gamma                109.127(2)
_cell_formula_units_Z            2
_cell_length_a                   15.8008(7)
_cell_length_b                   16.2412(11)
_cell_length_c                   19.6284(11)
_cell_measurement_temperature    296(2)
_cell_volume                     4263.5(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.958
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0894
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33433
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.663
_diffrn_reflns_theta_min         2.154
_exptl_absorpt_coefficient_mu    0.642
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_colour_primary    purple
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_refine_diff_density_max         2.380
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     887
_refine_ls_number_reflns         19085
_refine_ls_number_restraints     315
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1117P)^2^+7.9525P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1891
_refine_ls_wR_factor_ref         0.2160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12291
_reflns_number_total             19085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc04003a2.cif
_cod_data_source_block           w_sq
_cod_original_cell_volume        4263.5(4)
_cod_database_code               7124706
_shelxl_version_number           2013-2
_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, All O(H,H) groups
2. Restrained distances
 O12-H12A
 0.82 with sigma of 0.02
 O12-H12B
 0.82 with sigma of 0.02
3. 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
4. Uiso/Uaniso restraints and constraints
Uanis(F10) = Uanis(F7) = Uanis(F11) = Uanis(F12) = Uanis(F9) = Uanis(F8)
5.a Me refined with riding coordinates:
 C21(H21A,H21B,H21C), C4AA(H4AA,H4AB,H4AC), C16(H16A,H16B,H16C), C0AA(H0AA,
 H0AB,H0AC), C9AA(H9AA,H9AB,H9AC), C70(H70A,H70B,H70C)
5.b Aromatic/amide H refined with riding coordinates:
 C60(H60), C59(H59), C58(H58), C56(H56), C55(H55), C54(H54), C53(H53),
 C50(H50), C47(H47), C46(H46), C45(H45), C44(H44), C42(H42), C41(H41), C40(H40),
  C39(H39), C37(H37), C33(H33), C32(H32), C31(H31), C30(H30), C27(H27),
 C25(H25), C24(H24), C23(H23), C20(H20), C19(H19), C18(H18), C1AA(H1AA),
 C11(H11), C3AA(H3AA), C5(H5), C4(H4), C3(H3), C2AA(H2AA), C1(H1)
5.c Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C)
;
_shelx_fab_checksum              57124
_olex2_submission_special_instructions 'No special instructions were received'