Supramolecular Hybrids Based on Ru(II) Porphyrin and Octahedral Mo(II) Iodide Cluster
Volostnykh, Marina V.; Kirakosyan, Gayane; Sinelshchikova, Anna A.; Loboda, Polina; Dorovatovskii, Pavel; Maxim, Mihailov; Tsivadze, Aslan Yu; Sokolov, Maksim Nailyevich; Gorbunova, Yulia G.; Dalton Transactions  (2023) –; doi:10.1039/D3DT00251A

data_7712637
_publ_section_title
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 Supramolecular Hybrids Based on Ru(II) Porphyrin and Octahedral Mo(II)
 Iodide Cluster
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00251A
_journal_year                    2023
_chemical_formula_moiety
'C246 H168 I8 Mo6 N30 O18 Ru6, 2(C35 H26 N4 O2 Ru), 4(C3 D6 O), 2(C16 H33 N)'
_chemical_formula_sum            'C360 H292 D24 I8 Mo6 N40 O26 Ru8'
_chemical_formula_weight         8042.06
_chemical_name_common            CP6+2
_chemical_properties_physical    Photo-sensitive
_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
_audit_creation_date             2023-02-21
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-02-27 deposited with the CCDC.	2023-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                110.2710(10)
_cell_angle_beta                 109.4890(10)
_cell_angle_gamma                99.2040(10)
_cell_formula_units_Z            1
_cell_length_a                   21.1183(7)
_cell_length_b                   22.5011(7)
_cell_length_c                   24.4219(8)
_cell_measurement_reflns_used    4620
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      23.023
_cell_measurement_theta_min      2.314
_cell_volume                     9751.6(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX II area-detector diffractometer'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            164313
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.796
_exptl_absorpt_coefficient_mu    1.179
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0818 before and 0.0588 after correction.
The Ratio of minimum to maximum transmission is 0.8197.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             3992
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method 'heptane, acetone-d6'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         2.751
_refine_diff_density_min         -1.426
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2009
_refine_ls_number_reflns         35660
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1381
_refine_ls_R_factor_gt           0.0778
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1367P)^2^+70.8085P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20442
_reflns_number_total             35660
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00251a2.cif
_cod_data_source_block           mv715lt
_cod_database_code               7712637
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.650
_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, All O(H,H) groups
2. Restrained distances
 N51-C51 \\sim N51-C61 \\sim N51-C81 \\sim N51-C71
 with sigma of 0.04
 C51-C52 \\sim C52-C53 \\sim C53-C54 \\sim C61-C62 \\sim C62-C63 \\sim C63-C64
\\sim C71-C72 \\sim C72-C73
 \\sim C73-C74 \\sim C81-C82 \\sim C82-C83 \\sim C83-C84
 with sigma of 0.04
 C51-C53 \\sim C52-C54 \\sim C61-C63 \\sim C62-C64 \\sim C71-C73 \\sim C72-C74
\\sim C81-C83 \\sim C82-C84
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C132) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C230) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C231) \\sim Ueq, Uanis(C232) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C8) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O1(0.5) C1(0.5) D1A(0.5) D1B(0.5) D1C(0.5) C6(0.5) C10(0.5)
 D10A(0.5) D10B(0.5) D10C(0.5) O2(0.5) C2(0.5) C17(0.5) D17A(0.5) D17B(0.5)
 D17C(0.5) C18(0.5) D18A(0.5) D18B(0.5) D18C(0.5) O5(0.5) C3(0.5) D3A(0.5)
 D3B(0.5) D3C(0.5) C7(0.5) O15(0.5) C4(0.5) D4A(0.5) D4B(0.5) D4C(0.5) C5(0.5)
 C9(0.5) D9A(0.5) D9B(0.5) D9C(0.5) C8(0.5) D8A(0.5) D8B(0.5) D8C(0.5)
 Fixed X: H41A(0.80018) H41B(0.76946)
 Fixed Y: H41A(0.66619) H41B(0.71728)
 Fixed Z: H41A(0.71928) H41B(0.72789)
5.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C71(H71A,H71B), C81(H81A,H81B), C52(H52A,H52B), C62(H62A,
 H62B), C61(H61A,H61B), C73(H73A,H73B), C72(H72A,H72B), C63(H63A,H63B),
 C53(H53A,H53B), C83(H83A,H83B), C82(H82A,H82B)
5.b Me refined with riding coordinates:
 C115(H11A,H11B,H11C), C132(H13A,H13B,H13C), C215(H21A,H21B,H21C), C232(H23A,
 H23B,H23C), C315(H31A,H31B,H31C), C332(H33A,H33B,H33C), C415(H41C,H41D,H41E),
 C432(H43A,H43B,H43C), C17(D17A,D17B,D17C), C18(D18A,D18B,D18C), C84(H84A,H84B,
 H84C), C54(H54A,H54B,H54C), C74(H74A,H74B,H74C), C8(D8A,D8B,D8C)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C14(H14), C15(H15), C22(H22), C23(H23), C24(H24),
 C25(H25), C32(H32), C33(H33), C34(H34), C35(H35), C102(H102), C103(H103),
 C105(H105), C107(H107), C108(H108), C112(H112), C113(H113), C116(H116),
 C117(H117), C119(H119), C120(H120), C122(H122), C124(H124), C125(H125),
 C129(H129), C130(H130), C133(H133), C134(H134), C202(H202), C203(H203),
 C205(H205), C207(H207), C208(H208), C212(H212), C213(H213), C216(H216),
 C217(H217), C219(H219), C220(H220), C222(H222), C224(H224), C225(H225),
 C229(H229), C230(H230), C233(H233), C234(H234), C302(H302), C303(H303),
 C305(H305), C307(H307), C308(H308), C312(H312), C313(H313), C316(H316),
 C317(H317), C319(H319), C320(H320), C322(H322), C324(H324), C325(H325),
 C329(H329), C330(H330), C333(H333), C334(H334), C402(H402), C403(H403),
 C405(H405), C407(H407), C408(H408), C412(H412), C413(H413), C416(H416),
 C417(H417), C419(H419), C420(H420), C422(H422), C424(H424), C425(H425),
 C429(H429), C430(H430), C433(H433), C434(H434)
5.d Idealised Me refined as rotating group:
 C1(D1A,D1B,D1C), C10(D10A,D10B,D10C), C3(D3A,D3B,D3C), C4(D4A,D4B,D4C),
 C9(D9A,D9B,D9C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 653 electrons were 
found in a volume of 2231\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C3D6O] per Formula Unit 
which account for 662 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99171
_shelx_hkl_checksum              58465
_shelx_fab_checksum              61373
_olex2_submission_special_instructions 'No special instructions were received'