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_7130342
_publ_section_title
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 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 H156 N6 O66 Rh12'
_chemical_formula_sum            'C204 H156 N6 O66 Rh12'
_chemical_formula_weight         4982.26
_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             2022-06-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-06 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                   31.480(5)
_cell_length_b                   31.480(5)
_cell_length_c                   72.390(5)
_cell_measurement_reflns_used    5987
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.332
_cell_measurement_theta_min      2.390
_cell_volume                     62127(15)
_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)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Pilatus DECTRIS 6M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82653
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       80
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            170930
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        27.332
_diffrn_reflns_theta_max         27.332
_diffrn_reflns_theta_min         2.390
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    0.799
_exptl_crystal_description       needle
_exptl_crystal_F_000             14940
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.008
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.567
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         9423
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.565
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.1427
_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          0.3901
_refine_ls_wR_factor_ref         0.4292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5365
_reflns_number_total             9423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx_CCDC2
_cod_original_cell_volume        62127(20)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7130342
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C11I-C10I
 2.4 with sigma of 0.02
3. Rigid bond restraints
 C6P, C3P, C2P, C1P, N1P, C5P, C4P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2P, C6P, O1P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C9I, C12I, C11I, C10I
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Me refined with riding coordinates:
 C12I(H12A,H12B,H12D), C11I(H11A,H11B,H11D), C10I(H10A,H10B,H10D)
5.b Aromatic/amide H refined with riding coordinates:
 C7C(H7C), C15C(H15C), C16C(H16C), C14C(H14C), C12C(H12C), C11C(H11C),
 C10C(H10C), C5C(H5C), C4P(H4P), C1P(H1P), C5P(H5P), C3I(H3I), C3C(H3C),
 C2P(H2P), C7I(H7I), C4C(H4C), C5I(H5I)
5.c Fitted hexagon refined as free rotating group:
 C14C(C13C,C12C,C11C,C10C,C9C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23963
_shelx_hkl_checksum              54381
_shelx_fab_checksum              15096
_olex2_submission_special_instructions 'No special instructions were received'