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_7130336
_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         'C228 H264 N12 O66 Rh12'
_chemical_formula_sum            'C228 H264 N12 O66 Rh12'
_chemical_formula_weight         5463.42
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-07-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-22 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            3
_cell_length_a                   26.590
_cell_length_b                   26.590
_cell_length_c                   43.610
_cell_measurement_reflns_used    0.82656
_cell_measurement_temperature    100
_cell_measurement_theta_max      60
_cell_measurement_theta_min      1
_cell_volume                     26702.590
_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
_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     0.82653
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_unetI/netI     0.0802
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            64408
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.933
_diffrn_reflns_theta_max         24.933
_diffrn_reflns_theta_min         1.496
_exptl_absorpt_coefficient_mu    0.894
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.019
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             8352
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6603
_refine_ls_number_restraints     195
_refine_ls_restrained_S_all      1.401
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0806
_refine_ls_shift/su_max          0.002
_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          0.2688
_refine_ls_wR_factor_ref         0.2970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3800
_reflns_number_total             6603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           c12_anna
_cod_original_cell_volume        26702.6
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7130336
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.751
_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
2. Restrained distances
 N2A-C13A
 1.4 with sigma of 0.02
 C13A-N2A
 1.4 with sigma of 0.02
 C12I-C13I
 1.5 with sigma of 0.02
 C15I-C16I
 1.5 with sigma of 0.02
 N1A-N2A
 1 with sigma of 0.02
 C16I-C17I
 1.57 with sigma of 0.02
 C17I-C19I
 2.5 with sigma of 0.02
 C18I-C16I
 2 with sigma of 0.02
 C16I-C18I
 4 with sigma of 0.02
 C18I-C19I
 1.5 with sigma of 0.02
 C19I-C20I
 1.5 with sigma of 0.02
 C15I-C17I
 2.5 with sigma of 0.02
 C16I-C15I
 1.45 with sigma of 0.02
 C20I-C19I
 1.45 with sigma of 0.02
 C18I-C17I
 1.45 with sigma of 0.02
 C14I-C16I
 2.47 with sigma of 0.02
 C14I-C12I
 2.47 with sigma of 0.02
 C13I-C14I
 1.45 with sigma of 0.02
 C14I-C15I
 1.45 with sigma of 0.02
 C14I-C13I
 1.45 with sigma of 0.02
 C13I-C12I
 1.45 with sigma of 0.02
 C15I-C14I \\sim C14I-C13I
 with sigma of 0.02
3. Rigid bond restraints
 C14I, C15I, C16I, C18I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C18I, C20I, C19I, C17I, C16I, C15I, C14I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C19I, C18I, C17I, C16I, C15I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2A, C3A, C4A, C5A, C6A, C7A, N1A, N2A, C13A, C12A, C11A, C9A, C10A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1T, C2T, C3T, C4T, O1T
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim N2A \\sim N1A
\\sim C6A \\sim C5A \\sim C4A \\sim C3A \\sim C2A \\sim C7A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C20I) = Uanis(C19I) = Uanis(C18I) = Uanis(C17I) = Uanis(C16I) =
Uanis(C15I) = Uanis(C14I) = Uanis(C13I)
Uanis(C14I) = Uanis(C15I) = Uanis(C16I) = Uanis(C17I) = Uanis(C18I)
5. Rigid body (RIGU) restrains
 O5I, C9I, C10I, C11I, C12I, C13I, C14I, C15I
 with sigma for 1-2 distances of 0.1 and sigma for 1-3 distances of 0.1
 O5I, C9I, C10I, C11I, C12I, C13I, C14I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C4T(H4TA,H4TB), C10I(H10A,H10B), C1T(H1TA,H1TB), C9I(H9IA,H9IB), C11I(H11A,
 H11B), C12I(H12A,H12B), C14I(H14A,H14B), C16I(H16A,H16B), C3T(H3TA,H3TB),
 C2T(H2TA,H2TB), C15I(H15A,H15B), C13I(H13A,H13B), C18I(H18A,H18B), C17I(H17A,
 H17B), C19I(H19A,H19B)
6.b Me refined with riding coordinates:
 C20I(H20A,H20B,H20C)
6.c Aromatic/amide H refined with riding coordinates:
 C7I(H7I), C3I(H3I), C5I(H5I), C12A(H12C), C11A(H11C), C10A(H10C), C14A(H14C),
 C7A(H7A), C3A(H3A), C4A(H4A), C5A(H5A)
6.d Fitted hexagon refined as free rotating group:
 C13A(C12A,C11A,C10A,C9A,C14A), C6A(C7A,C2A,C3A,C4A,C5A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              88067
_shelx_hkl_checksum              10757
_shelx_fab_checksum              41947
_olex2_submission_special_instructions 'No special instructions were received'