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_7130339
_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         'C204 H120 N6 O66 Rh12'
_chemical_formula_sum            'C204 H120 N6 O66 Rh12'
_chemical_formula_weight         4945.97
_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             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            3
_cell_length_a                   29.1065(5)
_cell_length_b                   29.1065(5)
_cell_length_c                   56.2463(9)
_cell_measurement_reflns_used    11752
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.5719353465
_cell_measurement_theta_min      1.26187213704
_cell_volume                     41267.2(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Pilatus DECTRIS 6M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0810
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -58
_diffrn_reflns_number            100303
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.483
_diffrn_reflns_theta_max         25.483
_diffrn_reflns_theta_min         1.263
_exptl_absorpt_coefficient_mu    0.574
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    0.597
_exptl_crystal_description       prism
_exptl_crystal_F_000             7362
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         10826
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1372P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2286
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6173
_reflns_number_total             10826
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           abr638
_cod_original_cell_volume        41267.1(16)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7130339
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.961
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C15C-C6C
 1.3 with sigma of 0.02
 C13C-C16C
 1.4 with sigma of 0.02
 C16C-C15C
 1.5 with sigma of 0.02
 O2P-C6P \\sim O1P-C6P
 with sigma of 0.02
 C6C-C15C \\sim C16C-C13C
 with sigma of 0.02
 C16C-C14C \\sim C16C-C12C
 with sigma of 0.02
3. Restrained planarity
 O1P, C6P, O2P, C3P, C4P, C5P, N1P, C2P, C1P
 with sigma of 0.1
4. Rigid bond restraints
 C1P, N1P, C5P, C4P, C3P, C2P, C6P, O1P, O2P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6C, C7C, C13C, C16C, C15C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1C, C1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O4I, C12I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2I, C1I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C4C, C5C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3I, C4I, C5I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C7C \\sim C6C \\sim C5C \\sim C15C \\sim C16C \\sim C13C \\sim C14C \\sim C12C:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
6.a Aromatic/amide H refined with riding coordinates:
 C11I(H11I), C8I(H8I), C9I(H9I), C3I(H3I), C4I(H4I), C7I(H7I), C14C(H14C),
 C10C(H10C), C11C(H11C), C12C(H12C), C7C(H7C), C5C(H5C), C4C(H4C), C3C(H3C),
 C15C(H15C), C4P(H4P), C5P(H5P), C1P(H1P), C2P(H2P), C16C(H16C)
6.b Fitted hexagon refined as free rotating group:
 C11I(C6I,C5I,C8I,C9I,C10I), C14C(C9C,C10C,C11C,C12C,C13C), C7C(C6C,C5C,C4C,
 C3C,C2C), C4P(C5P,N1P,C1P,C2P,C3P)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              34688
_shelx_hkl_checksum              15316
_shelx_fab_checksum              95384
_olex2_submission_special_instructions 'No special instructions were received'