Development of a Ru-porphyrin-based supramolecular framework catalyst for styrene epoxidation.
Yoneda, Akira; Watanabe, Taito; Kosugi, Kento; Takahara, Teppei; Kusaka, Shinpei; Matsuda, Ryotaro; Saga, Yutaka; Kambe, Tetsuya; Kondo, Mio; Masaoka, Shigeyuki; Chemical communications (Cambridge, England) 60 (2024) 13939–13942; doi:10.1039/d4cc03868a

data_7133923
_publ_section_title
;
 Development of a Ru-porphyrin-based supramolecular framework catalyst for
 styrene epoxidation.
;
_journal_issue                   94
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              13939
_journal_page_last               13942
_journal_paper_doi               10.1039/d4cc03868a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C125 H92 N4 O2 Ru'
_chemical_formula_sum            'C125 H92 N4 O2 Ru'
_chemical_formula_weight         1783.09
_chemical_name_systematic
aquacarbonyl(5,10,15,20-tetrakis(4-(7-tert-butyl)-pyrene-2-yl)phenyl)porphyrinato)ruthenium(II)
_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     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc2kh6s2
_audit_creation_date             2024-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-21 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                112.717(5)
_cell_angle_beta                 94.736(5)
_cell_angle_gamma                95.806(5)
_cell_formula_units_Z            1
_cell_length_a                   7.8860(6)
_cell_length_b                   16.7298(10)
_cell_length_c                   19.9827(10)
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    122.8(6)
_cell_measurement_theta_max      24.4620
_cell_measurement_theta_min      2.0490
_cell_volume                     2398.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      8.00  37.00   0.50  230.00    --   10.88-107.00 -49.00   58
  2  \w    -55.00  -1.00   0.50  230.00    --  -12.67 107.00  48.00  108
  3  \w    -16.00  50.00   0.50  230.00    --   10.88 -99.00 150.00  132
  4  \w     -2.00  84.00   0.50  230.00    --   10.88  38.00 120.00  172
  5  \w    -63.00  40.00   0.50  230.00    --   10.88 -77.00-120.00  206
  6  \w     -6.00  80.00   0.50  230.00    --   10.88  57.00   0.00  172
  7  \w    -73.00 -46.00   0.50  230.00    --  -12.67-178.00-120.00   54
  8  \w    -72.00 -47.00   0.50  230.00    --  -12.67-178.00 -30.00   50
  9  \w    -87.00 -62.00   0.50  230.00    --  -12.67-178.00-150.00   50
 10  \w     -7.00  27.00   0.50  230.00    --  -12.67 -99.00 -60.00   68
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1580
_diffrn_reflns_av_unetI/netI     0.1864
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26546
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.053
_diffrn_reflns_theta_max         25.053
_diffrn_reflns_theta_min         2.050
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       needle
_exptl_crystal_F_000             930
_exptl_crystal_recrystallization_method
'slow evaporation of chloroform and MeCN solution, then dry'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8493
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0477P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4424
_reflns_number_total             8493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03868a2.cif
_cod_data_source_block           rubppycoh2o
_cod_depositor_comments
'Adding full bibliography for 7133922--7133923.cif.'
_cod_database_code               7133923
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.968
_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. Restrained distances
 C35B-C37B
 2.228 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C34: within 2A with sigma of 1.6 and sigma for terminal atoms of 3.2 within 2A
C34 \\sim C36B: within 2A with sigma of 1.6 and sigma for terminal atoms of 3.2
within 2A
C34 \\sim C35B: within 2A with sigma of 1.6 and sigma for terminal atoms of 3.2
within 2A
C34 \\sim C37B: within 2A with sigma of 1.6 and sigma for terminal atoms of 3.2
within 2A
Uanis(C34) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(Ru1) = Uanis(O2)
Uanis(C34) = Uanis(C36B) = Uanis(C37B)
Uanis(C36A) = Uanis(C35A) = Uanis(C37A)
Uanis(C34) = Uanis(C36B) = Uanis(C37B) = Uanis(C35B)
Uanis(C1) = Uanis(O1)
4. Others
 Fixed Sof: O1(0.5) O2(0.5) C1(0.5) C35A(0.75) H1A(0.75) H1C(0.75) H1B(0.75)
 C35B(0.25) H3C(0.25) H3B(0.25) H3A(0.25) C36B(0.25) H5B(0.25) H5A(0.25)
 H5C(0.25) C36A(0.75) H20A(0.75) H20C(0.75) H20B(0.75) C37B(0.25) H11A(0.25)
 H11B(0.25) H11C(0.25) C37A(0.75) H12A(0.75) H12B(0.75) H12C(0.75)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H01E), C4(H01B), C8(H00G), C9(H00B), C13(H01D), C14(H00M), C16(H00P),
 C17(H01A), C19(H017), C23(H00S), C24(H01G), C25(H01H), C29(H01J), C30(H01K),
 C31(H01T), C33(H01S), C39(H00W), C40(H012), C42(H00Y), C43(H015), C45(H014),
 C49(H016), C50(H010), C51(H00X), C55(H009), C56(H00F), C57(H01C), C59(H018)
5.b Idealised Me refined as rotating group:
 C35A(H1A,H1C,H1B), C35B(H3C,H3B,H3A), C36B(H5B,H5A,H5C), C36A(H20A,H20C,H20B),
  C37B(H11A,H11B,H11C), C37A(H12A,H12B,H12C), C61(H01O,H01M,H01N), C62(H01Q,
 H01P,H01R), C63(H01L,H01F,H01I)
;
_shelx_res_checksum              11127
_shelx_hkl_checksum              59725
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;