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_7130341
_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         'C252 H252 N6 O72 Rh12'
_chemical_formula_sum            'C252 H252 N6 O72 Rh12'
_chemical_formula_weight         5751.50
_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
_audit_creation_date             2022-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_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                   31.6843(5)
_cell_length_b                   31.6843(5)
_cell_length_c                   72.349(2)
_cell_measurement_reflns_used    11667
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.5825719627
_cell_measurement_theta_min      2.31646681651
_cell_volume                     62900(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.1340
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_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       72
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_number            134519
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.407
_diffrn_reflns_theta_max         24.407
_diffrn_reflns_theta_min         1.495
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.911
_exptl_crystal_description       cube
_exptl_crystal_F_000             17532
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.480
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.245
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     394
_refine_ls_number_reflns         7315
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.241
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.1105
_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          0.3237
_refine_ls_wR_factor_ref         0.3509
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4171
_reflns_number_total             7315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx_CCDC3
_cod_original_cell_volume        62900(3)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7130341
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.934
_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
 C12I-C11I
 1.67 with sigma of 0.02
 C12I-C13I
 1.67 with sigma of 0.02
 C14I-C13I
 1.67 with sigma of 0.02
 C9I-C10I
 1.67 with sigma of 0.02
 C15I-C16I
 1.67 with sigma of 0.02
 C10I-C11I
 1.67 with sigma of 0.02
 C17I-C16I
 1.67 with sigma of 0.02
 C19I-C18I
 1.67 with sigma of 0.02
 C14I-C15I
 1.67 with sigma of 0.02
 C11I-C10I
 1.67 with sigma of 0.02
 C19I-C20I
 1.67 with sigma of 0.02
 C17I-C18I
 1.67 with sigma of 0.02
 C12I-C10I
 3 with sigma of 0.02
 C11I-C13I
 3 with sigma of 0.02
 C13I-C15I
 3 with sigma of 0.02
 C17I-C19I
 3 with sigma of 0.02
 C18I-C20I
 3 with sigma of 0.02
 C14I-C16I
 3 with sigma of 0.02
 C15I-C17I
 3 with sigma of 0.02
 C12I-C14I
 3 with sigma of 0.02
 C10I-O5I
 3 with sigma of 0.02
 C11I-C9I
 3 with sigma of 0.02
 C3P-C6P
 1.39 with sigma of 0.02
 H17B-H17B_$1
 2.1 with sigma of 0.02
 H5I-H9IA
 2.1 with sigma of 0.02
3. Restrained planarity
 O1P, C6P, O2P, C3P, C2P, C4P, C5P, N1P, C1P
 with sigma of 0.1
4. Rigid bond restraints
 O1P, C6P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
Uanis(O5I) = Uanis(C9I) = Uanis(C10I) = Uanis(C11I) = Uanis(C12I) = Uanis(C13I)
= Uanis(C14I) = Uanis(C15I) = Uanis(C16I) = Uanis(C17I) = Uanis(C18I) =
Uanis(C19I) = Uanis(C20I)
6. Rigid body (RIGU) restrains
 C20I, C19I, C18I, C17I, C16I, C15I, C14I, C13I, C12I, C11I, C10I, C9I, O5I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7.a Secondary CH2 refined with riding coordinates:
 C9I(H9IA,H9IB), C11I(H11A,H11B), C12I(H12A,H12B), C13I(H13A,H13B), C14I(H14A,
 H14B), C15I(H15A,H15B), C16I(H16A,H16B), C10I(H10A,H10B), C17I(H17A,H17B),
 C18I(H18A,H18B), C19I(H19A,H19B)
7.b Me refined with riding coordinates:
 C20I(H20A,H20B,H20C)
7.c Aromatic/amide H refined with riding coordinates:
 C7I(H7I), C5I(H5I), C3I(H3I), C10C(H10C), C11C(H11C), C12C(H12C), C14C(H14C),
 C5C(H5C), C7C(H7C), C3C(H3C), C4C(H4C), C15C(H15C), C5P(H5P), C1P(H1P),
 C2P(H2P), C4P(H4P), C16C(H16C)
7.d Fitted hexagon refined as free rotating group:
 C2I(C7I,C6I,C5I,C4I,C3I), C9C(C10C,C11C,C12C,C13C,C14C), C5C(C6C,C7C,C2C,C3C,
 C4C), C5P(N1P,C1P,C2P,C3P,C4P)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              49470
_shelx_hkl_checksum              32862
_shelx_fab_checksum              5413
_olex2_submission_special_instructions 'No special instructions were received'