Synthesis and catalytic testing of the first hydrophilic derivative of Shvo's catalyst.
Diekamp, Justus; Schmidt, Annika; Holstein, Julian J.; Strohmann, Carsten; Seidensticker, Thomas; Chemical communications (Cambridge, England) 61 (2024) 117–120; doi:10.1039/d4cc04390a

data_7134018
_publ_section_title
;
 Synthesis and catalytic testing of the first hydrophilic derivative of
 Shvo's catalyst.
;
_journal_issue                   1
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              117
_journal_page_last               120
_journal_paper_doi               10.1039/d4cc04390a
_journal_volume                  61
_journal_year                    2024
_chemical_formula_moiety
'C136 H124 Na8 O48 Ru4 S8, 2(C H4 O), 0.5[CH4O]'
_chemical_formula_sum            'C139.25 H137 Na8 O51.25 Ru4 S8'
_chemical_formula_weight         3475.16
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-22 deposited with the CCDC.	2024-11-27 downloaded from the CCDC.
;
_cell_angle_alpha                80.3110(10)
_cell_angle_beta                 84.209(2)
_cell_angle_gamma                87.5740(10)
_cell_formula_units_Z            2
_cell_length_a                   14.6295(5)
_cell_length_b                   19.7444(6)
_cell_length_c                   26.6859(10)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.12
_cell_measurement_theta_min      2.33
_cell_volume                     7557.0(4)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker D8 VENTURE area detector'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CPAD PHOTON II area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'HELIOS mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            345772
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.726
_diffrn_reflns_theta_min         1.917
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.5640
_exptl_absorpt_correction_T_min  0.5114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0553 after correction.
The Ratio of minimum to maximum transmission is 0.9067.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             3549
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.154
_refine_diff_density_max         1.677
_refine_diff_density_min         -0.792
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2396
_refine_ls_number_reflns         42728
_refine_ls_number_restraints     2404
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0634P)^2^+21.9869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1612
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33828
_reflns_number_total             42728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04390a2.cif
_cod_data_source_block           mo_b3207_0m
_cod_depositor_comments          'Adding full bibliography for 7134018.cif.'
_cod_database_code               7134018
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.841
_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 C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 S2-O16 \\sim S2-O16A \\sim S2-O17 \\sim S2-O17A \\sim S2-O18 \\sim S2-O18A
 with sigma of 0.02
 S7-O31 \\sim S7-O31A \\sim S7-O32 \\sim S7-O32A \\sim S7-O33 \\sim S7-O33A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1N \\sim O41B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C1O \\sim O41: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(O41B)+Sof(H41B)+Sof(C1N)+Sof(H1NA)+Sof(H1NB)+Sof(H1NC)]+1*[Sof(O41A)+
 Sof(H41A)+Sof(C129)+Sof(H12P)+Sof(H12Q)+Sof(H12R)]+1*[Sof(O41)+Sof(H41)+
 Sof(C1O)+Sof(H1OA)+Sof(H1OB)+Sof(H1OC)]=1 with esd of 0
 Sof(Na3)=Sof(Na7)=Sof(O12A)=Sof(O31)=Sof(O32A)=Sof(O33A)=Sof(O35A)=Sof(O36A)=
 Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=Sof(H1C)=Sof(C1D)=Sof(H1D)=
 Sof(C1E)=Sof(H1E)=Sof(C94)=Sof(H94)=Sof(C95)=Sof(H95)=Sof(C97)=Sof(H97)=
 Sof(C98)=Sof(H98)=Sof(C105)=Sof(C106)=Sof(H106)=Sof(C107)=Sof(H107)=Sof(C108)=
 Sof(H108)=Sof(C109)=Sof(H109)=Sof(C110)=Sof(H110)=Sof(H40B)=Sof(C128)=
 Sof(H12M)=Sof(H12N)=Sof(H12O)=Sof(H54B)=Sof(C142)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=1-FVAR(1)
 Sof(Na3A)=Sof(Na7A)=Sof(O12)=Sof(O31A)=Sof(O32)=Sof(O33)=Sof(O35)=Sof(O36)=
 Sof(C1F)=Sof(C1G)=Sof(H1G)=Sof(C1H)=Sof(H1H)=Sof(C1I)=Sof(H1I)=Sof(C1J)=
 Sof(H1J)=Sof(C1K)=Sof(H1K)=Sof(C94A)=Sof(H94A)=Sof(C95A)=Sof(H95A)=Sof(C97A)=
 Sof(H97A)=Sof(C98A)=Sof(H98A)=Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=
 Sof(C102)=Sof(H102)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(H104)=Sof(H40A)=Sof(C1P)=
 Sof(H1PA)=Sof(H1PB)=Sof(H1PC)=Sof(H54A)=Sof(C146)=Sof(H14D)=Sof(H14E)=
 Sof(H14F)=FVAR(1)
 Sof(S1)=Sof(S4)=Sof(O13A)=Sof(O14A)=Sof(O15A)=Sof(O16)=Sof(O17)=Sof(O18)=
 Sof(O22)=Sof(O23)=Sof(O24)=Sof(O38)=Sof(H38)=Sof(O45)=Sof(H45)=Sof(O47)=
 Sof(H47)=Sof(C1L)=Sof(H1LA)=Sof(H1LB)=Sof(H1LC)=Sof(C1M)=Sof(H1MA)=Sof(H1MB)=
 Sof(H1MC)=Sof(H12D)=Sof(H12E)=Sof(H12F)=1-FVAR(2)
 Sof(S1A)=Sof(S4A)=Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16A)=Sof(O17A)=Sof(O18A)=
 Sof(O22A)=Sof(O23A)=Sof(O24A)=Sof(O38A)=Sof(H38A)=Sof(O45A)=Sof(H45A)=
 Sof(O47A)=Sof(H47A)=Sof(H12G)=Sof(H12H)=Sof(H12I)=Sof(C133)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C135)=Sof(H13J)=Sof(H13K)=Sof(H13L)=FVAR(2)
 Sof(O41B)=Sof(H41B)=Sof(C1N)=Sof(H1NA)=Sof(H1NB)=Sof(H1NC)=FVAR(3)
 Sof(O41A)=Sof(H41A)=Sof(C129)=Sof(H12P)=Sof(H12Q)=Sof(H12R)=FVAR(4)
 Sof(O41)=Sof(H41)=Sof(C1O)=Sof(H1OA)=Sof(H1OB)=Sof(H1OC)=FVAR(5)
 Fixed Sof: Na9(0.25) Na9A(0.25) O48(0.6) H48(0.6) O49(0.4) H49(0.4) O50(0.25)
 H50(0.25) C136(0.6) H13M(0.6) H13N(0.6) H13O(0.6) C137(0.4) H13P(0.4)
 H13Q(0.4) H13R(0.4) C138(0.25) H13S(0.25) H13T(0.25) H13U(0.25) O42(0.5)
 H42A(0.5) O52(0.5) H52A(0.5) C130(0.5) H13V(0.5) H13W(0.5) H13X(0.5) C140(0.5)
 H14G(0.5) H14H(0.5) H14I(0.5)
6.a Me refined with riding coordinates:
 C132(H13A,H13B,H13C), C137(H13P,H13Q,H13R), C130(H13V,H13W,H13X)
6.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C1B(H1B), C1C(H1C), C1D(H1D), C1E(H1E), C1G(H1G), C1H(H1H),
 C1I(H1I), C1J(H1J), C1K(H1K), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
 C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C25(H25), C26(H26), C28(H28), C29(H29), C36(H36), C37(H37A),
 C39(H39A), C40(H40), C42(H42), C43(H43), C44(H44A), C45(H45B), C46(H46A),
 C48(H48A), C49(H49A), C50(H50A), C51(H51), C52(H52), C54(H54), C55(H55),
 C57(H57), C58(H58), C65(H65), C66(H66), C68(H68), C69(H69), C71(H71), C72(H72),
  C73(H73), C74(H74), C75(H75), C77(H77), C78(H78), C79(H79), C80(H80),
 C81(H81), C83(H83), C84(H84), C86(H86), C87(H87), C94(H94), C94A(H94A),
 C95(H95), C95A(H95A), C97(H97), C97A(H97A), C98(H98), C98A(H98A), C100(H100),
 C101(H101), C102(H102), C103(H103), C104(H104), C106(H106), C107(H107),
 C108(H108), C109(H109), C110(H110), C112(H112), C113(H113), C115(H115),
 C116(H116)
6.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O4(H4), O37(H37), O38(H38), O38A(H38A), O44(H44), O45(H45),
 O45A(H45A), O46(H46), O47(H47), O47A(H47A), O48(H48), O49(H49), O50(H50),
 O40(H40B), O40(H40A), O41(H41), O41A(H41A), O41B(H41B), O42(H42A), O43(H43A),
 O52(H52A), O51(H51A), O54(H54B), O54(H54A)
6.d Idealised Me refined as rotating group:
 C1L(H1LA,H1LB,H1LC), C1M(H1MA,H1MB,H1MC), C125(H12A,H12B,H12C), C126(H12D,
 H12E,H12F), C126(H12G,H12H,H12I), C127(H12J,H12K,H12L), C133(H13D,H13E,H13F),
 C134(H13G,H13H,H13I), C135(H13J,H13K,H13L), C136(H13M,H13N,H13O), C138(H13S,
 H13T,H13U), C1N(H1NA,H1NB,H1NC), C1O(H1OA,H1OB,H1OC), C1P(H1PA,H1PB,H1PC),
 C128(H12M,H12N,H12O), C129(H12P,H12Q,H12R), C131(H13Y,HB,HC), C140(H14G,H14H,
 H14I), C139(H13Z,HD,HE), C141(H14J,H14K,H14L), C142(H14A,H14B,H14C), C146(H14D,
 H14E,H14F)
6.e Idealised tetrahedral OH refined as rotating group:
 O39(H39), O53(H53)
;
_shelx_res_checksum              65235
_olex2_submission_special_instructions 'No special instructions were received'