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_7130345
_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
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC03220A
_journal_year                    2022
_chemical_formula_moiety         'C174 H108 N6 O60 Rh12, 8(C4 H9 N O)'
_chemical_formula_sum            'C206 H182 N14 O68 Rh12'
_chemical_formula_weight         5176.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
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2022-05-31 deposited with the CCDC.	2022-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                99.5536(3)
_cell_angle_beta                 109.2065(3)
_cell_angle_gamma                113.9476(7)
_cell_formula_units_Z            1
_cell_length_a                   20.10034(7)
_cell_length_b                   21.47025(6)
_cell_length_c                   23.37885(8)
_cell_measurement_reflns_used    65242
_cell_measurement_temperature    100
_cell_measurement_theta_max      33.5385707343
_cell_measurement_theta_min      1.28303527884
_cell_volume                     8166.47(8)
_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 0.911
_diffrn_measured_fraction_theta_max 0.750
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0951
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 0.911
_diffrn_reflns_Laue_measured_fraction_max 0.750
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            103894
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.750
_diffrn_reflns_theta_full        29.731
_diffrn_reflns_theta_max         33.801
_diffrn_reflns_theta_min         1.287
_exptl_absorpt_coefficient_mu    0.971
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.053
_exptl_crystal_description       prism
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.493
_refine_diff_density_min         -2.024
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1268
_refine_ls_number_reflns         31293
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1650P)^2^+9.0151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2431
_refine_ls_wR_factor_ref         0.2478
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28306
_reflns_number_total             31293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx_CCDC5
_cod_original_cell_volume        8166.45(6)
_cod_database_code               7130345
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.860
_shelx_estimated_absorpt_t_min   0.845
_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
 H3DB_$1-H11I
 2.2 with sigma of 0.02
 C47C-C38C
 1.44 with sigma of 0.02
 C48C-C45C
 1.44 with sigma of 0.02
 C48C-C47C
 1.5 with sigma of 0.02
 C44C-C47C
 3.7 with sigma of 0.02
 C39C-C48C
 3.7 with sigma of 0.02
 H9P_$1-H8DC
 2.1 with sigma of 0.02
 C47C-C39C \\sim C47C-C37C
 with sigma of 0.02
 C47C-C38C \\sim C48C-C45C
 with sigma of 0.02
 C48C-C46C \\sim C48C-C44C
 with sigma of 0.02
3. Rigid bond restraints
 C39C, C34C, C35C, C36C, C37C, C38C, C47C, C48C, C45C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3D, N3D, C12D, C10D, C9D, C11D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O10C, C33C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C14P, C13P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O3D \\sim N3D \\sim C10D \\sim C12D \\sim C9D \\sim C11D: within 2A with sigma
of 0.04 and sigma for terminal atoms of 0.08
C47C \\sim C48C \\sim C38C \\sim C37C \\sim C36C \\sim C35C \\sim C34C \\sim
C39C \\sim C45C: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C11I) = Uanis(C12I) = Uanis(C13I)
Uanis(C16D) = Uanis(N4D) = Uanis(C14D) = Uanis(C13D) = Uanis(C15D) = Uanis(O4D)
Uanis(C48C) = Uanis(C47C)
Uanis(C21I) = Uanis(C20I) = Uanis(C19I)
5.a Me refined with riding coordinates:
 C8D(H8DA,H8DB,H8DC), C3D(H3DA,H3DB,H3DC), C7D(H7DA,H7DB,H7DC), C5D(H5DA,H5DB,
 H5DC), C9D(H9DA,H9DB,H9DC), C11D(H11A,H11B,H11D), C16D(H16A,H16B,H16D),
 C12D(H12A,H12B,H12D), C15D(H15A,H15B,H15D), C1D(H1DA,H1DB,H1DC), C13D(H13A,
 H13B,H13C)
5.b Aromatic/amide H refined with riding coordinates:
 C19C(H19C), C10P(H10P), C9P(H9P), C7I(H7I), C23I(H23I), C20C(H20C), C7C(H7C),
 C19I(H19I), C28C(H28C), C30C(H30C), C15C(H15C), C44C(H44C), C46C(H46C),
 C42C(H42C), C43C(H43C), C23C(H23C), C6P(H6P), C5P(H5P), C12I(H12I), C31C(H31C),
  C11P(H11P), C7P(H7P), C1P(H1P), C20I(H20I), C12P(H12P), C3C(H3C), C5I(H5I),
 C4C(H4C), C21C(H21C), C26C(H26C), C14C(H14C), C27C(H27C), C32C(H32C), C3I(H3I),
  C11I(H11I), C15I(H15I), C16C(H16C), C10C(H10C), C48C(H48C), C5C(H5C),
 C4P(H4P), C2P(H2P), C15P(H15P), C21I(H21I), C12C(H12C), C14P(H14P), C4I(H4I),
 C11C(H11C), C13I(H13I), C37C(H37C), C36C(H36C), C35C(H35C), C39C(H39C),
 C47C(H47C)
5.c Fitted hexagon refined as free rotating group:
 C44C(C45C,C46C,C41C,C42C,C43C), C37C(C36C,C35C,C34C,C39C,C38C)
5.d Idealised Me refined as rotating group:
 C4D(H4DA,H4DB,H4DC)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              44808
_shelx_hkl_checksum              55647
_shelx_fab_checksum              58119
_olex2_submission_special_instructions 'No special instructions were received'