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_7130344
_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 H144 N6 O72 Rh12'
_chemical_formula_sum            'C204 H144 N6 O72 Rh12'
_chemical_formula_weight         5066.16
_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             2022-05-16
_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                   31.4131(2)
_cell_length_b                   31.4131(2)
_cell_length_c                   72.4411(2)
_cell_measurement_reflns_used    23922
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.5127120153
_cell_measurement_theta_min      1.50239089797
_cell_volume                     61906.6(6)
_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      100.0
_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  0.0648
_diffrn_reflns_av_unetI/netI     0.0268
_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       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -73
_diffrn_reflns_number            142271
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.921
_diffrn_reflns_theta_max         24.921
_diffrn_reflns_theta_min         1.089
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.815
_exptl_crystal_description       prism
_exptl_crystal_F_000             15156
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.448
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.343
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         7642
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      1.343
_refine_ls_R_factor_all          0.1240
_refine_ls_R_factor_gt           0.1098
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_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          0.3219
_refine_ls_wR_factor_ref         0.3447
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5140
_reflns_number_total             7642
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           abr554
_cod_original_cell_volume        61906.6(8)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7130344
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.914
_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
 C10I-C11I
 1.4 with sigma of 0.02
 C3P-C6P
 1.5 with sigma of 0.02
 C11I-C12I
 1.4 with sigma of 0.02
 O5I-C9I
 1.4 with sigma of 0.02
 C9I-C10I
 1.4 with sigma of 0.02
 C9I-C11I
 2.5 with sigma of 0.02
 C10I-C12I
 2.5 with sigma of 0.02
3. Rigid bond restraints
 O1P, C6P, O2P, C3P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3C, C4C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13C, C16C, C15C, C6C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6I, C5I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O1P \\sim C6P \\sim O2P \\sim C3P: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C8C \\sim C9C: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C12I) = Uanis(C11I) = Uanis(C10I) = Uanis(C9I) = Uanis(O5I)
5. Rigid body (RIGU) restrains
 O1P, C6P, O2P, C3P
 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:
 C10I(H10A,H10B), C11I(H11A,H11B)
6.b Me refined with riding coordinates:
 C12I(H12A,H12B,H12D)
6.c Aromatic/amide H refined with riding coordinates:
 C7C(H7C), C14C(H14C), C10C(H10C), C12C(H12C), C16C(H16C), C3C(H3C), C1P(H1P),
 C2P(H2P), C5P(H5P), C15C(H15C), C3I(H3I), C7I(H7I), C5I(H5I), C4P(H4P),
 C11C(H11C), C5C(H5C), C4C(H4C)
6.d Fitted hexagon refined as free rotating group:
 C3I(C2I,C7I,C6I,C5I,C4I)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20401
_shelx_hkl_checksum              62770
_shelx_fab_checksum              95733
_olex2_submission_special_instructions 'No special instructions were received'