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_7133922
_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         'C127 H95 N5 O Ru, C H Cl3, 4(C2 H3 N)'
_chemical_formula_sum            'C136 H108 Cl3 N9 O Ru'
_chemical_formula_weight         2091.73
_chemical_name_common            Ru(BPPy)(CO)(MeCN)
_chemical_name_systematic
acetonitrilecarbonyl{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.cc2kh6t3
_audit_creation_date             2024-09-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-20 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                102.612(2)
_cell_angle_beta                 104.1350(10)
_cell_angle_gamma                93.6510(10)
_cell_formula_units_Z            2
_cell_length_a                   15.3821(2)
_cell_length_b                   16.7184(4)
_cell_length_c                   23.3719(3)
_cell_measurement_reflns_used    33179
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      31.0790
_cell_measurement_theta_min      1.7430
_cell_volume                     5644.16(18)
_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 0.837
_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     40.00  74.00   0.50   17.72    --   11.03-143.00  27.00   68
  2  \w     19.00  44.00   0.50   17.72    --   11.03-128.00-161.00   50
  3  \w    -68.00 -38.00   0.50   17.72    --  -12.83 128.00 -87.00   60
  4  \w    -63.00 -38.00   0.50   17.72    --  -12.83 143.00  83.00   50
  5  \w    -63.00  40.00   0.50   17.72    --   11.03 -77.00 120.00  206
  6  \w    -14.00  21.00   0.50   17.72    --   11.03 -99.00 -90.00   70
  7  \w     55.00  82.00   0.50   17.72    --   11.03-178.00  30.00   54
  8  \w    -10.00  82.00   0.50   17.72    --   11.03  57.00-120.00  184
  9  \w    -60.00  40.00   0.50   17.72    --   11.03 -77.00  30.00  200
 10  \w    -90.00 -45.00   0.50   17.72    --  -12.83-178.00 -30.00   90
 11  \w    -76.00 -45.00   0.50   17.72    --  -12.83-178.00-120.00   62
 12  \w    -69.00 -44.00   0.50   17.72    --  -12.83-178.00 120.00   50
 13  \w     -8.00  25.00   0.50   17.72    --  -12.83 -99.00-180.00   66
;
_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  0.0455
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            95711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.309
_diffrn_reflns_theta_min         1.733
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.813
_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_density_diffrn    1.231
_exptl_crystal_description       needle
_exptl_crystal_F_000             2180
_exptl_crystal_size_max          0.91
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.199
_refine_diff_density_min         -1.491
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1399
_refine_ls_number_reflns         30950
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1148
_refine_ls_R_factor_gt           0.0820
_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^)+(0.1574P)^2^+2.5478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21269
_reflns_number_total             30950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc03868a2.cif
_cod_data_source_block           rubppycomecn
_cod_depositor_comments
'Adding full bibliography for 7133922--7133923.cif.'
_cod_database_code               7133922
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.794
_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. Others
 Sof(C97A)=Sof(H97a)=Sof(H97b)=Sof(H97c)=Sof(C98A)=Sof(H98a)=Sof(H98b)=
 Sof(H98c)=Sof(C99A)=Sof(H99a)=Sof(H99b)=Sof(H99c)=1-FVAR(1)
 Sof(C97B)=Sof(H97d)=Sof(H97e)=Sof(H97f)=Sof(C98B)=Sof(H98d)=Sof(H98e)=
 Sof(H98f)=Sof(C99B)=Sof(H99d)=Sof(H99e)=Sof(H99f)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C136(H136)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C8(H8), C9(H9), C13(H13), C14(H14), C18(H18), C19(H19),
 C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C33(H33), C34(H34), C35(H35),
  C39(H39), C40(H40), C41(H41), C43(H43), C49(H49), C50(H50), C52(H52),
 C53(H53), C55(H55), C59(H59), C60(H60), C61(H61), C65(H65), C66(H66), C67(H67),
  C69(H69), C75(H75), C76(H76), C78(H78), C79(H79), C81(H81), C85(H85),
 C86(H86), C87(H87), C91(H91), C92(H92), C93(H93), C95(H95), C101(H101),
 C102(H102), C104(H104), C105(H105), C107(H107), C111(H111), C112(H112),
 C113(H113), C117(H117), C118(H118), C119(H119), C121(H121)
3.c Idealised Me refined as rotating group:
 C45(H45a,H45b,H45c), C46(H46a,H46b,H46c), C47(H47a,H47b,H47c), C71(H71a,H71b,
 H71c), C72(H72a,H72b,H72c), C73(H73a,H73b,H73c), C97A(H97a,H97b,H97c),
 C97B(H97d,H97e,H97f), C98A(H98a,H98b,H98c), C98B(H98d,H98e,H98f), C99A(H99a,
 H99b,H99c), C99B(H99d,H99e,H99f), C123(H12a,H12b,H12c), C124(H12d,H12e,H12f),
 C125(H12g,H12h,H12i), C127(H12j,H12k,H12l), C135(H13a,H13b,H13c), C131(H13d,
 H13e,H13f), C133(H13g,H13h,H13i), C129(H12m,H12n,H12o)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              61768
_shelx_hkl_checksum              46575
_shelx_fab_checksum              6994
_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
;