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_7712636
_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         'C246 H168 I8 Mo6 N30 O18 Ru6'
_chemical_formula_sum            'C246 H168 I8 Mo6 N30 O18 Ru6'
_chemical_formula_weight         6029.35
_chemical_name_common            CP6
_chemical_properties_physical    Photo-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-02-21
_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                 108.56(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.408(6)
_cell_length_b                   27.031(5)
_cell_length_c                   22.388(5)
_cell_measurement_reflns_used    21286
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      3.3
_cell_volume                     15724(6)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            86647
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         26.666
_diffrn_reflns_theta_min         2.012
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  0.955
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       prism
_exptl_crystal_F_000             5876
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetone, heptane'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.202
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         14683
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0618
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+17.6169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1813
_refine_ls_wR_factor_ref         0.2134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7215
_reflns_number_total             14683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00251a2.cif
_cod_data_source_block           mv716
_cod_original_cell_volume        15723(6)
_cod_database_code               7712636
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.863
_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. Rigid bond restraints
 O4, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, C57
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C58, C59
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C38, C37
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C41) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C57) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Fixed Sof: O4(0.5)
5.a Me refined with riding coordinates:
 C57(H57A,H57B,H57C), C22(H22A,H22B,H22C), C39(H39A,H39B,H39C)
5.b Aromatic/amide H refined with riding coordinates:
 C47(H47), C64(H64), C26(H26), C36(H36), C37(H37), C40(H40), C41(H41),
 C10(H10), C61(H61), C6(H6), C9(H9), C4(H4), C27(H27), C43(H43), C29(H29),
 C62(H62), C5(H5), C46(H46), C44(H44), C23(H23), C50(H50), C3(H3), C32(H32),
 C12(H12), C20(H20), C49(H49), C19(H19), C31(H31), C11(H11), C24(H24), C15(H15),
  C14(H14), C59(H59), C58(H58), C55(H55), C54(H54)
5.c Fitted hexagon refined as free rotating group:
 C35(C36,C37,C38,C40,C41), C53(C59,C58,C56,C55,C54)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 788 electrons were 
found in a volume of 788\%A^3^ in 1 void per Asymmetric Unit. 
This is consistent with the presence of 
0.5[C16H36N+], 0.5[CHCl3] per Asymmetric Unit 
which account for 6304 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32691
_shelx_hkl_checksum              21252
_shelx_fab_checksum              62344
_olex2_submission_special_instructions 'No special instructions were received'