Engineering a molecular ruthenium catalyst into three-dimensional metal covalent organic frameworks for efficient water oxidation.
Han, Wang-Kang; Liu, Yong; Feng, Jing-Dong; Yan, Xiaodong; Pang, Huan; Gu, Zhi-Guo; Chemical science 14 (2023) 11768–11774; doi:10.1039/d3sc03681b

data_1570056
_publ_section_title
;
 Engineering a molecular ruthenium catalyst into three-dimensional metal
 covalent organic frameworks for efficient water oxidation.
;
_journal_issue                   42
_journal_name_full               'Chemical science'
_journal_page_first              11768
_journal_page_last               11774
_journal_paper_doi               10.1039/d3sc03681b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C24 H16 Cl2 N4 O4 Ru, C2 H3 N'
_chemical_formula_sum            'C26 H19 Cl2 N5 O4 Ru'
_chemical_formula_weight         637.43
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-17
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2023-06-16 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                71.0740(10)
_cell_angle_beta                 84.6940(10)
_cell_angle_gamma                73.6690(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8691(3)
_cell_length_b                   11.2102(3)
_cell_length_c                   11.8287(3)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      57.011
_cell_measurement_theta_min      3.687
_cell_volume                     1308.34(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19503
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_min         1.820
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.6028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1128 before and 0.0465 after correction.
The Ratio of minimum to maximum transmission is 0.8024.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5293
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0300P)^2^+1.5966P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0780
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4845
_reflns_number_total             5293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03681b2.cif
_cod_data_source_block           11_sq
_cod_depositor_comments
'Adding full bibliography for 1570056--1570057.cif.'
_cod_database_code               1570056
_shelx_shelxl_version_number     2018/3
_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
2. Restrained distances
 O4-C24 = O5-C24
 1.2 with sigma of 0.01
 O5-C24
 1.2 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
C26 \\sim N5 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(C25) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(H24A)=Sof(O4)=1-FVAR(1)
 Sof(H24)=Sof(O5)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C6(H6), C8(H8), C4(H4), C22(H22), C15(H15), C16(H16), C20(H20),
 C12(H12), C3(H3), C9(H9), C11(H11), C1(H1), C14(H14), C23(H23), C24(H24),
 C24(H24A)
5.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              66364
_shelx_fab_checksum              16635
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'