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_7130338
_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         'C234 H252 N24 O60 Rh12'
_chemical_formula_sum            'C234 H252 N24 O60 Rh12'
_chemical_formula_weight         5595.50
_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             2022-05-16
_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            3
_cell_length_a                   33.9017(2)
_cell_length_b                   33.9017(2)
_cell_length_c                   23.6843(7)
_cell_measurement_reflns_used    10743
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.8397783612
_cell_measurement_theta_min      1.38736017375
_cell_volume                     23574.0(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Pilatus DECTRIS 6M'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0791
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            99905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        29.731
_diffrn_reflns_theta_max         33.399
_diffrn_reflns_theta_min         1.898
_exptl_absorpt_coefficient_mu    1.014
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       prism
_exptl_crystal_F_000             8532
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.319
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.137
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         12006
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1094
_refine_ls_R_factor_gt           0.0806
_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^)+(0.1648P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2342
_refine_ls_wR_factor_ref         0.2602
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6454
_reflns_number_total             12006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx(9)
_cod_original_cell_volume        23574.0(8)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7130338
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.897
_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
 C11I-C12I
 1.4 with sigma of 0.02
 C11I-C10I
 1.4 with sigma of 0.02
 C9P-C8P \\sim C9P-C7P \\sim C8P-C7P \\sim C7Q-C8Q \\sim C7Q-C9Q \\sim C8Q-C9Q
 with sigma of 0.04
 C6P-C3P \\sim C6P-C9P \\sim C6P-C8P \\sim C6P-C7P \\sim C6P-C7Q \\sim C6P-C8Q
\\sim C6P-C9Q
 with sigma of 0.02
3. Rigid bond restraints
 C12I, C11I, C10I, C9I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Rigid body (RIGU) restrains
 C7Q, C6P, C8Q, C9Q, C3P
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6P, C8P, C9P, C7P, C3P
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C7Q)=Sof(H7QA)=Sof(H7QB)=Sof(H7QC)=Sof(C8Q)=Sof(H8QA)=Sof(H8QB)=Sof(H8QC)=
 Sof(C9Q)=Sof(H9QA)=Sof(H9QB)=Sof(H9QC)=1-FVAR(1)
 Sof(C9P)=Sof(H9PA)=Sof(H9PB)=Sof(H9PC)=Sof(C8P)=Sof(H8PA)=Sof(H8PB)=Sof(H8PC)=
 Sof(C7P)=Sof(H7PA)=Sof(H7PB)=Sof(H7PC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C9I(H9IA,H9IB), C10I(H10B,H10C), C11I(H11B,H11C)
6.b Me refined with riding coordinates:
 C1D(H1DA,H1DB,H1DC), C4D(H4DA,H4DB,H4DC), C3D(H3DA,H3DB,H3DC), C9P(H9PA,H9PB,
 H9PC), C8P(H8PA,H8PB,H8PC), C7P(H7PA,H7PB,H7PC), C12I(H12B,H12C,H12D),
 C7Q(H7QA,H7QB,H7QC), C8Q(H8QA,H8QB,H8QC), C9Q(H9QA,H9QB,H9QC)
6.c Aromatic/amide H refined with riding coordinates:
 C7I(H7I), C3I(H3I), C14A(H14A), C5P(H5P), C4P(H4P), C5I(H5I), C7A(H7A),
 C10A(H10A), C1P(H1P), C2P(H2P), C3A(H3A), C11A(H11A), C12A(H12A), C5A(H5A),
 C4A(H4A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              33275
_shelx_hkl_checksum              83901
_shelx_fab_checksum              61667
_olex2_submission_special_instructions 'No special instructions were received'