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_7130343
_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         '2(C96 H54 N9 O33 Rh6), C3 H7 N O'
_chemical_formula_sum            'C195 H115 N19 O67 Rh12'
_chemical_formula_weight         5030.97
_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             2022-05-17
_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                87.892(2)
_cell_angle_beta                 68.779(2)
_cell_angle_gamma                77.069(2)
_cell_formula_units_Z            2
_cell_length_a                   22.9616(5)
_cell_length_b                   27.9645(4)
_cell_length_c                   29.9154(4)
_cell_measurement_reflns_used    19305
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.4609668583
_cell_measurement_theta_min      0.852548523248
_cell_volume                     17431.6(6)
_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 0.906
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.82656
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.906
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            188103
_diffrn_reflns_point_group_measured_fraction_full 0.906
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_theta_full        29.731
_diffrn_reflns_theta_max         29.884
_diffrn_reflns_theta_min         0.850
_exptl_absorpt_coefficient_mu    0.908
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.959
_exptl_crystal_description       prism
_exptl_crystal_F_000             4988
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.698
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2464
_refine_ls_number_reflns         57778
_refine_ls_number_restraints     451
_refine_ls_restrained_S_all      1.173
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.1123
_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          0.3103
_refine_ls_wR_factor_ref         0.3414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                32960
_reflns_number_total             57778
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03220a2.cif
_cod_data_source_block           shelx_CCDC4
_cod_original_cell_volume        17431.7(6)
_cod_database_code               7130343
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.868
_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
 C33P-C36P
 1.5 with sigma of 0.02
 N4A-C27A
 1.4 with sigma of 0.02
 N3A-C20A
 1.4 with sigma of 0.02
 N3A-N4A
 1.2 with sigma of 0.02
 C3P-C6P
 1.4 with sigma of 0.02
 C50I-C49I
 1.4 with sigma of 0.02
 C15P-C18P
 1.4 with sigma of 0.02
 C8A-C9A
 1.4 with sigma of 0.02
 N3A-C21A \\sim N3A-C19A
 with sigma of 0.02
 N4A-C28A \\sim N4A-C26A
 with sigma of 0.02
3. Restrained planarity
 O11P, C36P, O12P, C33P, C34P, C32P, C31P, N6P, C35P
 with sigma of 0.1
 O2P, C6P, O1P, C3P
 with sigma of 0.1
 C16A, C21A, C20A, N3A, C19A, C18A, C17A
 with sigma of 0.1
4. Rigid bond restraints
 C81A, C82A, C83A, C84A, C79A, C80A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C80A, C81A, C82A, C83A, C84A, C79A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C74A, C73A, C77A, C72A, C76A, C75A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25A, C26A, C27A, N3A, N4A, C20A, C18A, C19A, C21A, C16A, C17A, C28A, C23A,
 C24A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C54A, C55A, C56A, C51A, C52A, C53A, N8A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C15A, C16A, C17A, C18A, C19A, C20A, C21A, N4A, N3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O2P, O1P, C6P, C3P, C4P, C2P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12P, C36P, O11P, C33P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O12P, C36P, O11P, C33P, C32P, C31P, N6P, C35P, C34P
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C76A \\sim N11A \\sim C83A \\sim N12A: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
N8A \\sim C55A \\sim N7A \\sim C48A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C34P \\sim C33P \\sim C35P \\sim N6P \\sim C31P \\sim C32P: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim C51A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O12P \\sim C36P \\sim O11P \\sim C33P: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C20A \\sim N3A \\sim N4A \\sim C27A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C21A \\sim C20A \\sim C19A \\sim C18A \\sim C17A \\sim C16A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C28P \\sim C29P \\sim N5P \\sim C26P \\sim C27P \\sim C25P: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C3P \\sim C6P \\sim O1P \\sim O2P: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
O6P \\sim C18P \\sim O5P \\sim C15P: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C31P \\sim C32P \\sim N6P \\sim C35P \\sim C34P \\sim C33P \\sim C36P \\sim
O12P \\sim O11P: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
C76A \\sim C75A \\sim C74A \\sim C73A \\sim C72A \\sim C77A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C76A) = Uanis(N11A) = Uanis(N12A) = Uanis(C83A) = Uanis(C82A) =
Uanis(C81A) = Uanis(C80A) = Uanis(C79A) = Uanis(C84A)
Uanis(C20A) = Uanis(N3A) = Uanis(N4A) = Uanis(C27A)
Uanis(C2D) = Uanis(N1D) = Uanis(C1D) = Uanis(C3D) = Uanis(O1D)
6.a Me refined with riding coordinates:
 C2D(H2DA,H2DB,H2DC), C3D(H3DA,H3DB,H3DC)
6.b Aromatic/amide H refined with riding coordinates:
 C70A(H70A), C71I(H71I), C47I(H47I), C5A(H5A), C7I(H7I), C3I(H3I), C4I(H4I),
 C55I(H55I), C11I(H11I), C68A(H68A), C67A(H67A), C59I(H59I), C69I(H69I),
 C19P(H19P), C67I(H67I), C4A(H4A), C25P(H25P), C19I(H19I), C7A(H7A), C63A(H63A),
  C43I(H43I), C63I(H63I), C3A(H3A), C20P(H20P), C66A(H66A), C51I(H51I),
 C56I(H56I), C13P(H13P), C23I(H23I), C68I(H68I), C14A(H14A), C64I(H64I),
 C42A(H42A), C38A(H38A), C57I(H57I), C1D(H1D), C31I(H31I), C45A(H45A),
 C47A(H47A), C16P(H16P), C23P(H23P), C59A(H59A), C31A(H31A), C45I(H45I),
 C20I(H20I), C11P(H11P), C7P(H7P), C8P(H8P), C10P(H10P), C17P(H17P), C35I(H35I),
  C52I(H52I), C84A(H84A), C54A(H54A), C53A(H53A), C52A(H52A), C56A(H56A),
 C14P(H14P), C5P(H5P), C26P(H26P), C27I(H27I), C49A(H49A), C8I(H8I), C39I(H39I),
  C61A(H61A), C35A(H35A), C22P(H22P), C44I(H44I), C46A(H46A), C60A(H60A),
 C21I(H21I), C9I(H9I), C33A(H33A), C40I(H40I), C40A(H40A), C12A(H12A),
 C10A(H10A), C26A(H26A), C25A(H25A), C24A(H24A), C28A(H28A), C15I(H15I),
 C28I(H28I), C39A(H39A), C32A(H32A), C11A(H11A), C4P(H4P), C80A(H80A),
 C29P(H29P), C75A(H75A), C74A(H74A), C73A(H73A), C77A(H77A), C16I(H16I),
 C2P(H2P), C1P(H1P), C28P(H28P), C33I(H33I), C32I(H32I), C82A(H82A), C34P(H34P),
  C32P(H32P), C31P(H31P), C35P(H35P), C81A(H81A), C21A(H21A), C17A(H17A),
 C18A(H18A), C19A(H19A)
6.c Fitted hexagon refined as free rotating group:
 C7I(C2I,C3I,C4I,C5I,C6I), C11P(N2P,C7P,C8P,C9P,C10P), C55A(C54A,C53A,C52A,
 C51A,C56A), C27A(C26A,C25A,C24A,C23A,C28A), C76A(C75A,C74A,C73A,C72A,C77A),
 C34P(C33P,C32P,C31P,N6P,C35P), C20A(C21A,C16A,C17A,C18A,C19A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82385
_shelx_hkl_checksum              75111
_shelx_fab_checksum              63838
_olex2_submission_special_instructions 'No special instructions were received'