A porous metal‒organic cage constructed from dirhodium paddle-wheels: synthesis, structure and catalysis
Chen, Lianfen; Yang, Tao; Cui, Hao; Cai, Tao; Zhang, Li; Su, Cheng-Yong; Journal of Materials Chemistry A 3 (2015) 20201–; doi:10.1039/C5TA05592J

data_7236112
_publ_section_title
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 A porous metal--organic cage constructed from dirhodium paddle-wheels:
 synthesis, structure and catalysis
;
_journal_issue                   40
_journal_name_full               'Journal of Materials Chemistry A'
_journal_page_first              20201
_journal_paper_doi               10.1039/C5TA05592J
_journal_volume                  3
_journal_year                    2015
_chemical_formula_moiety
'C104 H70 N2 O20 Rh4, 3(C4 H9 N O), 2(C2.5 H4.5 N O0.5), 2(H2 O), 2(O)'
_chemical_formula_sum            'C121 H110 N7 O28 Rh4'
_chemical_formula_weight         2521.80
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-05 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                72.966(7)
_cell_angle_beta                 73.450(6)
_cell_angle_gamma                68.665(6)
_cell_formula_units_Z            1
_cell_length_a                   14.3649(9)
_cell_length_b                   15.5751(10)
_cell_length_c                   16.3871(12)
_cell_measurement_reflns_used    7184
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      64.8320
_cell_measurement_theta_min      3.3340
_cell_volume                     3199.2(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector_area_resol_mean 10.6525
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20800
_diffrn_reflns_theta_full        65.37
_diffrn_reflns_theta_max         65.37
_diffrn_reflns_theta_min         3.12
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.685
_exptl_absorpt_correction_T_max  0.7995
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1289
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.427
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         10596
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1049P)^2^+6.2428P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1697
_refine_ls_wR_factor_ref         0.1986
_reflns_number_gt                7175
_reflns_number_total             10596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ta05592j2.cif
_cod_data_source_block           1
_cod_database_code               7236112
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H54A,H54B,H54C} of C54, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H56A,H56B,H56C} of C56, {H57A,H57B,H57C} of C57, {H1AA,
  H1AB,H1AC} of C1A, {H1BA,H1BB,H1BC} of C1B, {H1CA,H1CB,H1CC} of C1C, {H49A,
  H49B,H49C} of C49, {H51A,H51B,H51C} of C51, {H53A,H53B,H53C} of C53, {H58A,
  H58B,H58C} of C58, {H60A,H60B,H60C} of C60, {H61A,H61B,H61C} of C61, All O(H,
  H) groups
2. Restrained distances
 C1C-C1D
 1.53 with sigma of 0.04
3. Others
 Fixed Sof: O13(0.5) N2(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5)
 H1BA(0.5) H1BB(0.5) H1BC(0.5) C1C(0.5) H1CA(0.5) H1CB(0.5) H1CC(0.5) C1D(0.5)
 O14(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C60(0.5) H60A(0.5) H60B(0.5)
 H60C(0.5) C61(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
4.a Free rotating group:
 O11(H11A,H11B)
4.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C11(H11), C12(H12), C13(H13), C15(H15), C18(H18),
 C19(H19), C20(H20), C22(H22), C26(H26), C27(H27), C28(H28), C30(H30), C36(H36),
  C37(H37), C38(H38), C39(H39), C42(H42), C43(H43), C44(H44), C46(H46)
4.d Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C1A(H1AA,H1AB,
 H1AC), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,H1CC), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C53(H53A,H53B,H53C), C58(H58A,H58B,H58C), C60(H60A,H60B,H60C),
 C61(H61A,H61B,H61C)
;
_olex2_submission_special_instructions 'No special instructions were received'