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_7130337
_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 H168 N18 O72 Rh12'
_chemical_formula_sum            'C204 H168 N18 O72 Rh12'
_chemical_formula_weight         5258.47
_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                   28.4941(2)
_cell_length_b                   28.4941(2)
_cell_length_c                   46.4950(5)
_cell_measurement_reflns_used    19212
_cell_measurement_temperature    100
_cell_measurement_theta_max      21.2618816321
_cell_measurement_theta_min      1.40307696532
_cell_volume                     32692.4(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            55567
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.067
_diffrn_reflns_theta_max         22.067
_diffrn_reflns_theta_min         2.590
_exptl_absorpt_coefficient_mu    0.730
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.801
_exptl_crystal_description       prism
_exptl_crystal_F_000             7902
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.268
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.486
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5693
_refine_ls_number_restraints     398
_refine_ls_restrained_S_all      2.509
_refine_ls_R_factor_all          0.1821
_refine_ls_R_factor_gt           0.1742
_refine_ls_shift/su_max          0.000
_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          0.4732
_refine_ls_wR_factor_ref         0.5059
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4592
_reflns_number_total             5693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        32692.4(6)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7130337
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.924
_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
 N1A-C6A
 1.4 with sigma of 0.02
 C4I-C8I
 2.8 with sigma of 0.02
 C9I-O5I
 2.8 with sigma of 0.02
 C4I-O5I
 1.4 with sigma of 0.02
 O5I-C10I
 4.5 with sigma of 0.02
 C8I-C10I
 2.8 with sigma of 0.02
 N2A-C13A
 1.4 with sigma of 0.02
 N1A-C13A
 2.1 with sigma of 0.02
 C6A-N2A
 2.1 with sigma of 0.02
 C9I-C11I
 2.8 with sigma of 0.02
 C10I-C12I
 2.8 with sigma of 0.02
 C11I-C13I
 2.8 with sigma of 0.02
 N1A-N2A
 1.2 with sigma of 0.02
 C9I-C12I
 4.5 with sigma of 0.02
 C13I-C10I
 4.5 with sigma of 0.02
 C6P-C3P
 1.5 with sigma of 0.02
 C8I-O5I
 1.5 with sigma of 0.02
 C9I-C10I
 1.54 with sigma of 0.02
 C11I-C12I
 1.54 with sigma of 0.02
 C10I-C11I
 1.54 with sigma of 0.02
 C12I-C13I
 1.54 with sigma of 0.02
 C8I-C9I
 1.54 with sigma of 0.02
 O5I-C8I
 1.54 with sigma of 0.02
 O5I-C8I \\sim C9I-C8I \\sim C9I-C10I \\sim C11I-C10I
 with sigma of 0.02
 O5I-C5I \\sim O5I-C3I
 with sigma of 0.02
 C11I-C10I \\sim C11I-C12I \\sim C13I-C12I
 with sigma of 0.02
 O2P-C6P \\sim O1P-C6P
 with sigma of 0.02
 N2A-C14A \\sim N2A-C12A
 with sigma of 0.02
 N1A-C7A \\sim N1A-C5A
 with sigma of 0.02
 O2I-C1I \\sim O1I-C1I
 with sigma of 0.02
3. Restrained planarity
 C4I, O5I, C5I, C3I
 with sigma of 0.1
 O1P, C6P, O2P, C3P
 with sigma of 0.1
4. Rigid bond restraints
 C13I, C12I, C11I, C10I, C9I, C8I, O5I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O1P, C6P, O2P, C2P, C3P, C4P, C1P, N1P, C5P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C9A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C7A, C6A
 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
 C6A, C7A, C3A, C2A, C4A, C5A, N1A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1A, N2A, C13A, C6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3A, C8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13A, C14A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1I, C2I, C3I, C4I, C5I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13A, C12A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C8I \\sim O5I \\sim C4I: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C13I \\sim C12I \\sim C11I \\sim C10I \\sim C9I \\sim C8I \\sim O5I: within 2A
with sigma of 0.04 and sigma for terminal atoms of 0.08
O1P \\sim C6P \\sim O2P \\sim C3P: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O2A \\sim C1A \\sim O1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim
C7A \\sim N1A \\sim N2A \\sim C13A \\sim C12A \\sim C11A \\sim C10A \\sim C9A
\\sim C8A \\sim O4A \\sim O3A \\sim C14A: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O4I \\sim C7I: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3I \\sim C2I \\sim C4I \\sim C5I \\sim C6I \\sim C1 \\sim C1I \\sim O1I \\sim
O2I \\sim C7I \\sim O4I \\sim O3I: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C5I \\sim C4I \\sim C3I \\sim C2I \\sim C1I: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C13I) = Uanis(C12I) = Uanis(C11I) = Uanis(C10I) = Uanis(C9I) = Uanis(C8I)
= Uanis(O5I)
Uanis(C1P) = Uanis(C2P)
6. Rigid body (RIGU) restrains
 C13I, C12I, C11I, C10I, C9I, C8I, 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:
 C11I(H11A,H11B), C10I(H10A,H10B), C8I(H8IA,H8IB), C9I(H9IA,H9IB), C12I(H12A,
 H12B)
7.b Me refined with riding coordinates:
 C13I(H13A,H13B,H13C)
7.c Aromatic/amide H refined with riding coordinates:
 C5I(H5I), C3I(H3I), C1(H1), C5P(H5P), C1P(H1P), C2P(H2P), C4P(H4P), C7A(H7A),
 C5A(H5A), C4A(H4A), C3A(H3A), C14A(H14A), C12A(H12C), C11A(H11C), C10A(H10C)
7.d Fitted hexagon refined as free rotating group:
 C6I(C5I,C4I,C3I,C2I,C1), C5P(N1P,C1P,C2P,C3P,C4P), C7A(C6A,C5A,C4A,C3A,C2A),
 C9A(C14A,C13A,C12A,C11A,C10A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32704
_shelx_hkl_checksum              98135
_shelx_fab_checksum              6232
_olex2_submission_special_instructions 'No special instructions were received'