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_7712635
_publ_section_title
;
 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
'C40 H29 N5 O Ru, 1.561(C0.745 Cl2.235 D0.745), 0.333(C1 Cl3)'
_chemical_formula_sum            'C41.5 H29 Cl4.49 D1.16 N5 O Ru'
_chemical_formula_weight         876.26
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-17
_audit_creation_method
;
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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   15.1883(4)
_cell_length_b                   15.1883(4)
_cell_length_c                   85.428(4)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.46
_cell_volume                     17066.7(10)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       121
_diffrn_reflns_limit_l_min       -116
_diffrn_reflns_number            74663
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.554
_diffrn_reflns_theta_min         2.457
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8276
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1477 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.8276.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             7965
_exptl_crystal_recrystallization_method 'CDCL3, piridine'
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.851
_refine_diff_density_min         -2.844
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         5828
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0689P)^2^+176.9631P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1614
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4868
_reflns_number_total             5828
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00251a2.cif
_cod_data_source_block           hex_0m
_cod_original_cell_volume        17066.7(11)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_original_formula_sum        'C41.50 H29 Cl4.49 D1.16 N5 O Ru'
_cod_database_code               7712635
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Others
 Sof(Cl2A)=1-FVAR(1)
 Sof(D24A)=0.33333*(1-FVAR(2))
 Sof(D24)=0.33333*FVAR(2)
 Sof(Cl2)=FVAR(1)
 Sof(Cl1)=1-FVAR(2)
 Sof(C22)=Sof(D22)=0.33333*(1-FVAR(3))
 Fixed Sof: C12(0.8333) H12(0.8333) C13(0.8333) H13(0.8333) C16(0.8333)
 H16(0.8333) C16A(0.1667) H16A(0.1667) C17(0.8333) H17(0.8333) C17A(0.1667)
 H17A(0.1667) Cl4(0.1667) C25(0.1667) C12A(0.1667) H12A(0.1667) C13A(0.1667)
 H13A(0.1667)
2.a Ternary CH refined with riding coordinates:
 C22(D22), C24(D24), C24(D24A)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C7(H7), C8(H8), C10(H10), C12(H12), C13(H13), C16(H16),
 C16A(H16A), C17(H17), C17A(H17A), C19(H19), C20(H20), C21(H21), C12A(H12A),
 C13A(H13A)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              13787
_shelx_hkl_checksum              141
_shelx_fab_checksum              13965
_olex2_submission_special_instructions 'No special instructions were received'