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_1570057
_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         'C48 H36 Cl2 N8 Ru, 2(C3 H7 N O)'
_chemical_formula_sum            'C54 H50 Cl2 N10 O2 Ru'
_chemical_formula_weight         1043.01
_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             2022-12-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-16 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                83.406(2)
_cell_angle_beta                 80.168(2)
_cell_angle_gamma                65.193(2)
_cell_formula_units_Z            4
_cell_length_a                   12.1419(5)
_cell_length_b                   14.3036(6)
_cell_length_c                   31.1469(13)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    193.00
_cell_measurement_theta_max      58.89
_cell_measurement_theta_min      3.16
_cell_volume                     4832.5(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2019)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.00
_diffrn_detector                 CPAD
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_monochromator  'Helios Multi-layer Optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0568
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            69057
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.468
_diffrn_reflns_theta_min         2.508
_diffrn_source                   MetalJet
_diffrn_source_current           2.86
_diffrn_source_power             0.19937059999999998
_diffrn_source_type              'Liquid Metal source'
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.731
_exptl_absorpt_correction_T_max  0.7518
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0895 before and 0.0632 after correction.
The Ratio of minimum to maximum transmission is 0.8190.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             2154
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.785
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         21259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0807P)^2^+16.7773P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1807
_refine_ls_wR_factor_ref         0.1958
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15652
_reflns_number_total             21259
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03681b2.cif
_cod_data_source_block           221217_wqangz_158574_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1570056--1570057.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C108 H101 Cl4 N20 O4 Ru2'
_cod_original_formula_weight         2087.02
_cod_original_formula_moiety
'C48 H37 Cl2 N8 Ru, C48 H36 Cl2 N8 Ru, 4(C3 H7 N O)'
_cod_original_formula_units_Z            2
_cod_database_code               1570057
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.718
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N5(H5), C62(H62), C38(H38), C41(H41), C9(H9), C17(H17), C39(H39), C35(H35),
 C33(H33), C63(H63), C89(H89), C55(H55), C14(H14), C34(H34), C57(H57), C59(H59),
  C11(H11), C83(H83), C42(H42), C86(H86), C65(H65), C31(H31), C81(H81),
 C82(H82), C58(H58), C66(H66), C10(H10), C15(H15), C18(H18), C87(H87), C90(H90),
  C53(H53), C7(H7), C29(H29), C20(H20), C26(H26), C24(H24), C25(H25), C49(H49),
 C69(H69), C48(H48), C21(H21), C47(H47), C52(H52), C28(H28), C96(H96), C68(H68),
  C70(H70), C44(H44), C92(H92), C46(H46), C22(H22), C23(H23), C94(H94),
 C45(H45), C79(H79), C93(H93), C72(H72), C95(H95), C108(H108), C27(H27),
 C71(H71), C51(H51), C50(H50), C1(H1), C2(H2), C5(H5A), C3(H3), C75(H75),
 C102(H102), C77(H77), C105(H105), C99(H99), C76(H76), C4(H4), C73(H73),
 C74(H74)
2.b Idealised Me refined as rotating group:
 C100(H10G,H10H,H10I), C107(H10A,H10B,H10C), C103(H10M,H10N,H10O), C97(H97A,
 H97B,H97C), C106(H10D,H10E,H10F), C104(H10P,H10Q,H10R), C101(H10J,H10K,H10L),
 C98(H98A,H98B,H98C)
;
_shelx_res_checksum              51319
_olex2_submission_special_instructions 'No special instructions were received'
_site                            XU