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_7130346
_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         'C216 H180 N6 O72 Rh12'
_chemical_formula_sum            'C216 H180 N6 O72 Rh12'
_chemical_formula_weight         5246.57
_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
_atom_sites_solution_primary     iterative
_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                   31.2593(3)
_cell_length_b                   31.2593(3)
_cell_length_c                   73.3075(10)
_cell_measurement_reflns_used    41354
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.8980311871
_cell_measurement_theta_min      1.50694442051
_cell_volume                     62035.1(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 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  0.0930
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       86
_diffrn_reflns_limit_l_min       -86
_diffrn_reflns_number            213203
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.090
_diffrn_reflns_theta_max         29.090
_diffrn_reflns_theta_min         1.515
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.843
_exptl_crystal_description       prism
_exptl_crystal_F_000             15804
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         11763
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0695
_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^)+(0.1667P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2399
_refine_ls_wR_factor_ref         0.2525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7368
_reflns_number_total             11763
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx_CCDC6
_cod_original_cell_volume        62035.1(15)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7130346
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.913
_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
 C14I-C12I
 2.639 with sigma of 0.02
 C11I-C13I
 2.639 with sigma of 0.02
 C10I-C12I
 2.7 with sigma of 0.02
 O5I-C10I
 2.7 with sigma of 0.02
 C13I-C11I
 2.7 with sigma of 0.02
 C11I-C9I
 2.7 with sigma of 0.02
 C10I-C9I
 1.7 with sigma of 0.02
 C14I-C13I
 1.7 with sigma of 0.02
 C13I-C14I \\sim C13I-C12I \\sim C12I-C11I \\sim C10I-C11I \\sim C9I-C10I
 with sigma of 0.02
3. Rigid bond restraints
 C14I, C13I, C12I, C11I, O5I, C9I, C10I
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C14I) = Uanis(C13I) = Uanis(C12I) = Uanis(C11I) = Uanis(C10I)
5.a Secondary CH2 refined with riding coordinates:
 C10I(H10A,H10B), C9I(H9IA,H9IB), C11I(H11A,H11B), C13I(H13A,H13B), C12I(H12A,
 H12B)
5.b Me refined with riding coordinates:
 C14I(H14A,H14B,H14D)
5.c Aromatic/amide H refined with riding coordinates:
 C7C(H7C), C14C(H14C), C7I(H7I), C5C(H5C), C2P(H2P), C3C(H3C), C1P(H1P),
 C3I(H3I), C15C(H15C), C5I(H5I), C4C(H4C), C5P(H5P), C16C(H16C), C10C(H10C),
 C4P(H4P), C12C(H12C), C11C(H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15038
_shelx_hkl_checksum              89388
_shelx_fab_checksum              99278
_olex2_submission_special_instructions 'No special instructions were received'