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_7130340
_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         'C186 H150 N18 O54 Rh12'
_chemical_formula_sum            'C186 H150 N18 O54 Rh12'
_chemical_formula_weight         4736.15
_chemical_name_systematic        het-Rh-MOP-1
_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             2022-05-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-31 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   31.163
_cell_length_b                   31.163
_cell_length_c                   69.154
_cell_measurement_reflns_used    4367
_cell_measurement_temperature    100
_cell_measurement_theta_max      60
_cell_measurement_theta_min      1
_cell_volume                     58160.276
_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
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0673
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            131593
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.672
_diffrn_reflns_theta_max         24.672
_diffrn_reflns_theta_min         1.520
_exptl_absorpt_coefficient_mu    0.809
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'reddish red'
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.811
_exptl_crystal_description       cube
_exptl_crystal_F_000             14184
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.088
_refine_diff_density_max         1.074
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.366
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         6990
_refine_ls_number_restraints     233
_refine_ls_restrained_S_all      1.362
_refine_ls_R_factor_all          0.1108
_refine_ls_R_factor_gt           0.1002
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3216
_refine_ls_wR_factor_ref         0.3418
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4750
_reflns_number_total             6990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        58160.2
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7130340
_shelx_shelxl_version_number     2018/3
_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
 H10A-H10A_$1
 2.1 with sigma of 0.02
 C8P-C9P \\sim C9P-C7P \\sim C7Q-C9Q \\sim C8Q-C9Q
 with sigma of 0.04
 C6P-C3P \\sim C6P-C8P \\sim C6P-C9P \\sim C6P-C7P \\sim C6P-C7Q \\sim C6P-C8Q
\\sim C6P-C9Q
 with sigma of 0.02
3. Rigid bond restraints
 C6P, C8P, C9P, C7P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4A, C5A, C6A, C2A, C7A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1I, C2I, C3I, C4I, C5I, C6I, C7I, C8I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3I, C8I, O4I, C6I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C11A, C12A, C10A, C13A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C4A \\sim C5A \\sim C6A \\sim C7A \\sim C2A \\sim C3A: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C11A \\sim C12A \\sim C10A \\sim C9A \\sim C13A: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C2A \\sim C1A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C10A) = Uanis(C11A) = Uanis(C12A)
5. Rigid body (RIGU) restrains
 C4A, C5A, C6A, C7A, C2A, C3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3P, C6P, C8Q, C7Q, C9Q
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3P, C6P, C8Q, C9Q, C7Q
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3P, C8P, C9P, C6P, C7P
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C7Q)=Sof(H7QA)=Sof(H7QB)=Sof(H7QC)=Sof(C8Q)=Sof(H8QA)=Sof(H8QB)=Sof(H8QC)=
 Sof(C9Q)=Sof(H9QA)=Sof(H9QB)=Sof(H9QC)=1-FVAR(1)
 Sof(C8P)=Sof(H8PA)=Sof(H8PB)=Sof(H8PC)=Sof(C9P)=Sof(H9PA)=Sof(H9PB)=Sof(H9PC)=
 Sof(C7P)=Sof(H7PA)=Sof(H7PB)=Sof(H7PC)=FVAR(1)
7.a Me refined with riding coordinates:
 C8P(H8PA,H8PB,H8PC), C9P(H9PA,H9PB,H9PC), C7P(H7PA,H7PB,H7PC), C7Q(H7QA,H7QB,
 H7QC), C8Q(H8QA,H8QB,H8QC), C9Q(H9QA,H9QB,H9QC)
7.b Aromatic/amide H refined with riding coordinates:
 C1P(H1P), C2P(H2P), C4P(H4P), C5P(H5P), C7I(H7I), C5I(H5I), C4I(H4I),
 C3I(H3I), C12A(H12A), C14A(H14A), C10A(H10A), C11A(H11A), C5A(H5A), C7A(H7A),
 C3A(H3A), C4A(H4A)
7.c Fitted hexagon refined as free rotating group:
 C1P(C2P,C3P,C4P,C5P,N1P), C2I(C7I,C6I,C5I,C4I,C3I), C12A(C13A,C14A,C9A,C10A,
 C11A), C5A(C6A,C7A,C2A,C3A,C4A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74036
_shelx_hkl_checksum              17385
_shelx_fab_checksum              67300
_olex2_submission_special_instructions 'No special instructions were received'