Synthesis of the Two Isomers of Heteroleptic Rh12L6L’6 Metal-Organic Polyhedra by Screening of Complementary Linkers
Broto-Ribas, Anna; Gutiérrez, Susana; Imaz, Inhar; Carné-Sánchez, Arnau; Gándara, Felipe; Juanhuix, Judith; Maspoch, Daniel; Chemical Communications  (2022) –; doi:10.1039/D2CC03220A

data_7130335
_publ_section_title
;
 Synthesis of the Two Isomers of Heteroleptic Rh12L6L&#x2019;6
 Metal-Organic Polyhedra by Screening of Complementary Linkers
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03220A
_journal_year                    2022
_chemical_formula_moiety
'C174 H162 N18 O60 Rh12, 2(C3 H7 N O), [+ solvents]'
_chemical_formula_sum            'C180 H176 N20 O62 Rh12'
_chemical_formula_weight         4846.32
_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     dual
_audit_creation_date             2021-07-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-08 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                98.356(5)
_cell_angle_beta                 109.317(5)
_cell_angle_gamma                109.104(4)
_cell_formula_units_Z            1
_cell_length_a                   19.1839(14)
_cell_length_b                   19.3591(14)
_cell_length_c                   21.9788(17)
_cell_measurement_reflns_used    4367
_cell_measurement_temperature    150
_cell_measurement_theta_max      60
_cell_measurement_theta_min      1
_cell_volume                     6978.3(10)
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1814
_diffrn_reflns_av_unetI/netI     0.2072
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45605
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        50.882
_diffrn_reflns_theta_max         50.882
_diffrn_reflns_theta_min         2.222
_diffrn_source                   Cu
_exptl_absorpt_coefficient_mu    6.108
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_description       prism
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   1
_exptl_transmission_factor_min   0.7544
_refine_diff_density_max         1.463
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1190
_refine_ls_number_reflns         14581
_refine_ls_number_restraints     470
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1575
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1135P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1990
_refine_ls_wR_factor_ref         0.2417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6823
_reflns_number_total             14581
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           1_a_res_in_p-1
_cod_original_cell_volume        6978.3(9)
_cod_database_code               7130335
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
'SADABS-2016/2 (Bunker,2016/2) was used for absortion correction. wR2(int)'
_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. Restrained distances
 C21I-C16I \\sim C21I-C24I \\sim C21I-C23I \\sim C21I-C22I \\sim C21I-C22J
\\sim C21I-C23J \\sim C21I-
 C24J
 with sigma of 0.02
 C9I-C10I \\sim C9I-C4I \\sim C9I-C12I \\sim C9I-C11I \\sim C9I-C11J \\sim
C9I-C12J \\sim C9I-C10J
 with sigma of 0.02
 C34J-C35J \\sim C34J-C36J \\sim C35J-C36J \\sim C34I-C35I \\sim C34I-C36I
\\sim C35I-C36I
 with sigma of 0.04
 C33J-C34J \\sim C33J-C35J \\sim C33J-C36J \\sim C33J-C28I \\sim C33J-C34I
\\sim C33J-C35I \\sim C33J-
 C36I
 with sigma of 0.02
 C34I-C35I \\sim C34I-C36I \\sim C35I-C36I
 with sigma of 0.04
 C10I-C12I \\sim C12I-C11I \\sim C11J-C12J \\sim C12J-C10J
 with sigma of 0.04
3. Rigid bond restraints
 O4D, C10D, N4D, C11D, C12D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C36I, C33J, C36J, C35I, C35J, C34I, C34J, C28I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10A, C29A, C30A, O9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4A, C8A, O3A, C9A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9D, N3D, C8D, C7D, O3D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C22I \\sim C22J \\sim C21I \\sim C23I \\sim C24I \\sim C24J \\sim C23J: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O4D \\sim C10D \\sim N4D \\sim C11D \\sim C12D: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C36J \\sim C33J \\sim C35J \\sim C34I \\sim C34J \\sim C35I \\sim C36I \\sim
C28I: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
Uanis(C1D) = Uanis(N1D) = Uanis(C3D) = Uanis(C2D) = Uanis(O1D)
Uanis(C7I) = Uanis(C2I) = Uanis(C3I) = Uanis(C6I) = Uanis(C4I) = Uanis(C8I)
Uanis(C25I) = Uanis(O9I) = Uanis(C26I) = Uanis(O10I)
Uanis(C22J) = Uanis(C21I) = Uanis(C23J) = Uanis(C24J)
Uanis(C35J) = Uanis(C33J) = Uanis(C36J)
Uanis(C6D) = Uanis(N2D) = Uanis(C5D) = Uanis(C4D) = Uanis(O2D)
5. Rigid body (RIGU) restrains
 C23J, C22J, C24J, C21I, C16I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C11I, C10I, C12I, C9I, C4I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22I, C23I, C21I, C24I, C16I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10J, C11J, C12J, C9I, C4I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34I, C36I, C35I, C33J, C28I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C34J, C36J, C35J, C33J, C28I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C11J)=Sof(H11E)=Sof(H11F)=Sof(H11G)=Sof(C12J)=Sof(H12E)=Sof(H12F)=
 Sof(H12G)=Sof(C10J)=Sof(H10E)=Sof(H10F)=Sof(H10G)=1-FVAR(1)
 Sof(C10I)=Sof(H10B)=Sof(H10C)=Sof(H10D)=Sof(C12I)=Sof(H12B)=Sof(H12C)=
 Sof(H12D)=Sof(C11I)=Sof(H11B)=Sof(H11C)=Sof(H11D)=FVAR(1)
 Fixed Sof: C34J(0.27875) H34A(0.27875) H34B(0.27875) H34C(0.27875)
 C35J(0.27875) H35B(0.27875) H35C(0.27875) H35D(0.27875) C36J(0.27875)
 H36A(0.27875) H36B(0.27875) H36C(0.27875) C24I(0.73335) H24B(0.73335)
 H24C(0.73335) H24D(0.73335) C23I(0.73335) H23A(0.73335) H23B(0.73335)
 H23C(0.73335) C22I(0.73335) H22A(0.73335) H22B(0.73335) H22C(0.73335)
 C34I(0.72125) H34D(0.72125) H34E(0.72125) H34F(0.72125) C35I(0.72125)
 H35E(0.72125) H35F(0.72125) H35G(0.72125) C36I(0.72125) H36D(0.72125)
 H36E(0.72125) H36F(0.72125) C22J(0.26665) H22D(0.26665) H22E(0.26665)
 H22F(0.26665) C23J(0.26665) H23D(0.26665) H23E(0.26665) H23F(0.26665)
 C24J(0.26665) H24E(0.26665) H24F(0.26665) H24G(0.26665)
7.a Me refined with riding coordinates:
 C12D(H12H,H12I,H12J), C11D(H11H,H11I,H11J), C2D(H2DA,H2DB,H2DC), C3D(H3DA,
 H3DB,H3DC), C5D(H5DA,H5DB,H5DC), C6D(H6DA,H6DB,H6DC), C8D(H8DA,H8DB,H8DC),
 C9D(H9DA,H9DB,H9DC), C34J(H34A,H34B,H34C), C35J(H35B,H35C,H35D), C36J(H36A,
 H36B,H36C), C10I(H10B,H10C,H10D), C12I(H12B,H12C,H12D), C11I(H11B,H11C,H11D),
 C24I(H24B,H24C,H24D), C23I(H23A,H23B,H23C), C22I(H22A,H22B,H22C), C34I(H34D,
 H34E,H34F), C35I(H35E,H35F,H35G), C36I(H36D,H36E,H36F), C22J(H22D,H22E,H22F),
 C23J(H23D,H23E,H23F), C24J(H24E,H24F,H24G), C11J(H11E,H11F,H11G), C12J(H12E,
 H12F,H12G), C10J(H10E,H10F,H10G)
7.b Aromatic/amide H refined with riding coordinates:
 C14A(H14A), C31A(H31A), C17I(H17I), C21A(H21A), C42A(H42A), C28A(H28A),
 C7A(H7A), C3I(H3I), C19I(H19I), C27I(H27I), C25A(H25A), C17A(H17A), C35A(H35A),
  C15I(H15I), C26A(H26A), C3A(H3A), C29I(H29I), C33A(H33A), C38A(H38A),
 C11A(H11A), C12A(H12A), C31I(H31I), C40A(H40A), C24A(H24A), C19A(H19A),
 C7I(H7I), C32A(H32A), C10A(H10A), C39A(H39A), C18A(H18A), C5I(H5I), C5A(H5A),
 C4A(H4A), C10D(H10H), C1D(H1D), C4D(H4D), C7D(H7D)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33519
_shelx_hkl_checksum              10591
_shelx_fab_checksum              21110
_olex2_submission_special_instructions 'No special instructions were received'