#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:52:15 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301804 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/55/2215593.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2215593
loop_
_publ_author_name
'Franco, Jimmy U.'
'Olmstead, Marilyn M.'
'Hammons, Justin C.'
_publ_section_title
Tetra-μ₂-acetato-κ⁸O:O'-bis{[1-(1-adamantyliminiomethyl)-2-naphtholato-κO]rhodium(II)}
_journal_coeditor_code           LH2508
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2606
_journal_page_last               m2607
_journal_paper_doi               10.1107/S1600536807046302
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Rh2 (C2 H3 O2)4 (C21 H23 N O)2]'
_chemical_formula_moiety         'C50 H58 N2 O10 Rh2'
_chemical_formula_sum            'C50 H58 N2 O10 Rh2'
_chemical_formula_weight         1052.80
_chemical_name_systematic
;
Tetra-μ₂-acetato-κ⁸O:O'-bis{[1-(1-adamantyliminomethyl)-
2-naphthol-\kO]rhodium(II)}
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.160(2)
_cell_angle_beta                 101.800(2)
_cell_angle_gamma                110.470(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5631(13)
_cell_length_b                   11.8424(16)
_cell_length_c                   11.8849(16)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.7
_cell_measurement_theta_min      3.1
_cell_volume                     1131.4(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELXTL (Sheldrick, 1994)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            30719
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.02
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.812
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Bruker, 2007)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.243
_refine_diff_density_min         -1.359
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0386
_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/[σ²(Fo²)+5.1888P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1114
_reflns_number_gt                5378
_reflns_number_total             5714
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            lh2508.cif
_cod_data_source_block           I
_cod_database_code               2215593
_cod_database_fobs_code          2215593
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Rh Rh1 0.03312(4) 0.07891(3) 0.45399(3) 0.01078(9) Uani d . 1
O O1 -0.1137(4) 0.1462(3) 0.5242(3) 0.0181(6) Uani d . 1
O O2 -0.1574(4) -0.0572(3) 0.2973(3) 0.0172(6) Uani d . 1
O O3 0.1782(4) 0.0040(3) 0.3903(3) 0.0167(6) Uani d . 1
O O4 0.2190(4) 0.2066(3) 0.6167(3) 0.0174(6) Uani d . 1
O O5 0.1100(4) 0.2411(3) 0.3856(3) 0.0163(6) Uani d . 1
N N1 0.2639(4) 0.4913(3) 0.4931(3) 0.0126(6) Uani d . 1
H H1 0.229(6) 0.420(5) 0.500(5) 0.013(12) Uiso d . 1
C C1 0.0905(5) 0.2486(4) 0.2782(4) 0.0138(8) Uani d . 1
C C2 -0.0022(5) 0.1327(4) 0.1631(4) 0.0137(7) Uani d . 1
H H2 -0.0487 0.0492 0.1668 0.016 Uiso calc R 1
C C3 -0.0240(5) 0.1408(4) 0.0501(4) 0.0149(8) Uani d . 1
H H3 -0.0881 0.0627 -0.0234 0.018 Uiso calc R 1
C C4 0.0458(5) 0.2625(4) 0.0370(4) 0.0137(7) Uani d . 1
C C5 0.0267(5) 0.2650(4) -0.0832(4) 0.0191(9) Uani d . 1
H H5 -0.0342 0.1852 -0.1556 0.023 Uiso calc R 1
C C6 0.0950(5) 0.3812(5) -0.0971(4) 0.0224(9) Uani d . 1
H H6 0.0811 0.3821 -0.1782 0.027 Uiso calc R 1
C C7 0.1860(5) 0.4990(4) 0.0113(4) 0.0203(8) Uani d . 1
H H7 0.2326 0.5800 0.0031 0.024 Uiso calc R 1
C C8 0.2074(5) 0.4973(4) 0.1279(4) 0.0167(8) Uani d . 1
H H8 0.2715 0.5776 0.1993 0.020 Uiso calc R 1
C C9 0.1380(5) 0.3811(4) 0.1462(4) 0.0137(7) Uani d . 1
C C10 0.1576(5) 0.3739(4) 0.2688(4) 0.0119(7) Uani d . 1
C C11 0.2387(5) 0.4898(4) 0.3803(4) 0.0145(7) Uani d . 1
H H11 0.2773 0.5718 0.3727 0.017 Uiso calc R 1
C C12 0.3360(5) 0.6120(4) 0.6110(4) 0.0129(7) Uani d . 1
C C13 0.4989(5) 0.7094(4) 0.6205(4) 0.0147(8) Uani d . 1
H H13A 0.4867 0.7366 0.5492 0.018 Uiso calc R 1
H H13B 0.5712 0.6666 0.6166 0.018 Uiso calc R 1
C C14 0.5699(5) 0.8310(4) 0.7452(4) 0.0163(8) Uani d . 1
H H14 0.6757 0.8949 0.7517 0.020 Uiso calc R 1
C C15 0.5894(5) 0.7881(4) 0.8553(4) 0.0170(8) Uani d . 1
H H15A 0.6635 0.7470 0.8540 0.020 Uiso calc R 1
H H15B 0.6347 0.8658 0.9356 0.020 Uiso calc R 1
C C16 0.4272(5) 0.6893(4) 0.8450(4) 0.0162(8) Uani d . 1
H H16 0.4409 0.6612 0.9163 0.019 Uiso calc R 1
C C17 0.3573(5) 0.5682(4) 0.7201(4) 0.0154(8) Uani d . 1
H H17A 0.4296 0.5255 0.7166 0.018 Uiso calc R 1
H H17B 0.2534 0.5037 0.7137 0.018 Uiso calc R 1
C C18 0.3131(5) 0.7544(4) 0.8501(4) 0.0183(8) Uani d . 1
H H18A 0.2085 0.6911 0.8437 0.022 Uiso calc R 1
H H18B 0.3564 0.8313 0.9309 0.022 Uiso calc R 1
C C19 0.2936(5) 0.7986(4) 0.7411(4) 0.0160(8) Uani d . 1
H H19 0.2208 0.8420 0.7445 0.019 Uiso calc R 1
C C20 0.4564(5) 0.8958(4) 0.7494(4) 0.0179(8) Uani d . 1
H H20A 0.4428 0.9235 0.6786 0.022 Uiso calc R 1
H H20B 0.5021 0.9751 0.8285 0.022 Uiso calc R 1
C C21 0.2217(5) 0.6765(4) 0.6165(4) 0.0143(8) Uani d . 1
H H21A 0.1176 0.6130 0.6109 0.017 Uiso calc R 1
H H21B 0.2047 0.7026 0.5449 0.017 Uiso calc R 1
C C22 0.1874(5) -0.0912(4) 0.4156(4) 0.0144(7) Uani d . 1
C C23 0.2955(5) -0.1445(4) 0.3671(4) 0.0207(9) Uani d . 1
H H23A 0.2345 -0.2388 0.3146 0.031 Uiso calc R 1
H H23B 0.3819 -0.1308 0.4380 0.031 Uiso calc R 1
H H23C 0.3402 -0.0985 0.3173 0.031 Uiso calc R 1
C C24 0.2413(5) 0.1683(4) 0.7049(4) 0.0153(8) Uani d . 1
C C25 0.3815(5) 0.2619(5) 0.8237(4) 0.0240(9) Uani d . 1
H H25A 0.3459 0.2701 0.8961 0.036 Uiso calc R 1
H H25B 0.4281 0.3484 0.8204 0.036 Uiso calc R 1
H H25C 0.4613 0.2280 0.8315 0.036 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O2 Rh1 O1 . . 89.35(12)
O2 Rh1 O4 . . 176.06(12)
O1 Rh1 O4 . . 90.08(12)
O2 Rh1 O3 . . 91.00(12)
O1 Rh1 O3 . . 176.25(12)
O4 Rh1 O3 . . 89.31(12)
O2 Rh1 O5 . . 97.98(11)
O1 Rh1 O5 . . 91.01(11)
O4 Rh1 O5 . . 85.92(11)
O3 Rh1 O5 . . 92.64(11)
O2 Rh1 Rh1 . 2_556 87.16(8)
O1 Rh1 Rh1 . 2_556 87.71(9)
O4 Rh1 Rh1 . 2_556 88.93(9)
O3 Rh1 Rh1 . 2_556 88.58(9)
O5 Rh1 Rh1 . 2_556 174.69(8)
C22 O1 Rh1 2_556 . 119.3(3)
C24 O2 Rh1 2_556 . 119.9(2)
C22 O3 Rh1 . . 118.0(3)
C24 O4 Rh1 . . 118.0(3)
C1 O5 Rh1 . . 135.9(3)
C11 N1 C12 . . 124.9(3)
C11 N1 H1 . . 118(3)
C12 N1 H1 . . 117(3)
O5 C1 C2 . . 121.2(4)
O5 C1 C10 . . 121.0(4)
C2 C1 C10 . . 117.8(4)
C3 C2 C1 . . 121.2(4)
C3 C2 H2 . . 119.4
C1 C2 H2 . . 119.4
C2 C3 C4 . . 122.6(4)
C2 C3 H3 . . 118.7
C4 C3 H3 . . 118.7
C5 C4 C9 . . 120.0(4)
C5 C4 C3 . . 120.5(4)
C9 C4 C3 . . 119.5(4)
C6 C5 C4 . . 121.1(4)
C6 C5 H5 . . 119.5
C4 C5 H5 . . 119.5
C5 C6 C7 . . 118.9(4)
C5 C6 H6 . . 120.6
C7 C6 H6 . . 120.6
C8 C7 C6 . . 120.5(4)
C8 C7 H7 . . 119.8
C6 C7 H7 . . 119.8
C7 C8 C9 . . 122.4(4)
C7 C8 H8 . . 118.8
C9 C8 H8 . . 118.8
C8 C9 C4 . . 117.1(4)
C8 C9 C10 . . 124.5(4)
C4 C9 C10 . . 118.3(4)
C11 C10 C1 . . 118.8(4)
C11 C10 C9 . . 120.6(4)
C1 C10 C9 . . 120.6(4)
N1 C11 C10 . . 124.2(4)
N1 C11 H11 . . 117.9
C10 C11 H11 . . 117.9
N1 C12 C17 . . 106.9(3)
N1 C12 C21 . . 109.2(3)
C17 C12 C21 . . 109.3(3)
N1 C12 C13 . . 111.5(3)
C17 C12 C13 . . 109.2(3)
C21 C12 C13 . . 110.7(3)
C12 C13 C14 . . 109.4(3)
C12 C13 H13A . . 109.8
C14 C13 H13A . . 109.8
C12 C13 H13B . . 109.8
C14 C13 H13B . . 109.8
H13A C13 H13B . . 108.2
C20 C14 C15 . . 109.1(3)
C20 C14 C13 . . 109.0(3)
C15 C14 C13 . . 109.5(3)
C20 C14 H14 . . 109.7
C15 C14 H14 . . 109.7
C13 C14 H14 . . 109.7
C16 C15 C14 . . 109.7(3)
C16 C15 H15A . . 109.7
C14 C15 H15A . . 109.7
C16 C15 H15B . . 109.7
C14 C15 H15B . . 109.7
H15A C15 H15B . . 108.2
C15 C16 C17 . . 109.6(3)
C15 C16 C18 . . 109.7(4)
C17 C16 C18 . . 109.5(3)
C15 C16 H16 . . 109.3
C17 C16 H16 . . 109.3
C18 C16 H16 . . 109.3
C12 C17 C16 . . 109.1(3)
C12 C17 H17A . . 109.9
C16 C17 H17A . . 109.9
C12 C17 H17B . . 109.9
C16 C17 H17B . . 109.9
H17A C17 H17B . . 108.3
C19 C18 C16 . . 109.2(3)
C19 C18 H18A . . 109.8
C16 C18 H18A . . 109.8
C19 C18 H18B . . 109.8
C16 C18 H18B . . 109.8
H18A C18 H18B . . 108.3
C18 C19 C20 . . 110.1(3)
C18 C19 C21 . . 108.6(3)
C20 C19 C21 . . 109.3(3)
C18 C19 H19 . . 109.6
C20 C19 H19 . . 109.6
C21 C19 H19 . . 109.6
C14 C20 C19 . . 110.2(3)
C14 C20 H20A . . 109.6
C19 C20 H20A . . 109.6
C14 C20 H20B . . 109.6
C19 C20 H20B . . 109.6
H20A C20 H20B . . 108.1
C12 C21 C19 . . 109.2(3)
C12 C21 H21A . . 109.8
C19 C21 H21A . . 109.8
C12 C21 H21B . . 109.8
C19 C21 H21B . . 109.8
H21A C21 H21B . . 108.3
O1 C22 O3 2_556 . 126.4(4)
O1 C22 C23 2_556 . 116.8(4)
O3 C22 C23 . . 116.8(4)
C22 C23 H23A . . 109.5
C22 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C22 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
O2 C24 O4 2_556 . 126.0(4)
O2 C24 C25 2_556 . 116.3(4)
O4 C24 C25 . . 117.7(4)
C24 C25 H25A . . 109.5
C24 C25 H25B . . 109.5
H25A C25 H25B . . 109.5
C24 C25 H25C . . 109.5
H25A C25 H25C . . 109.5
H25B C25 H25C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Rh1 O2 . 2.043(3) ?
Rh1 O1 . 2.042(3) ?
Rh1 O4 . 2.043(3) ?
Rh1 O3 . 2.044(3) ?
Rh1 O5 . 2.250(3) y
Rh1 Rh1 2_556 2.3983(7) y
O1 C22 2_556 1.263(5) ?
O2 C24 2_556 1.268(5) ?
O3 C22 . 1.275(5) ?
O4 C24 . 1.268(5) ?
O5 C1 . 1.286(5) y
N1 C11 . 1.306(5) y
N1 C12 . 1.489(5) ?
N1 H1 . 0.83(5) ?
C1 C2 . 1.444(5) ?
C1 C10 . 1.445(6) y
C2 C3 . 1.353(6) y
C2 H2 . 0.9500 ?
C3 C4 . 1.431(6) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.413(6) ?
C4 C9 . 1.423(5) ?
C5 C6 . 1.377(6) ?
C5 H5 . 0.9500 ?
C6 C7 . 1.413(6) ?
C6 H6 . 0.9500 ?
C7 C8 . 1.366(6) ?
C7 H7 . 0.9500 ?
C8 C9 . 1.406(6) ?
C8 H8 . 0.9500 ?
C9 C10 . 1.462(5) y
C10 C11 . 1.415(5) y
C11 H11 . 0.9500 ?
C12 C17 . 1.536(5) ?
C12 C21 . 1.538(5) ?
C12 C13 . 1.538(5) ?
C13 C14 . 1.542(5) ?
C13 H13A . 0.9900 ?
C13 H13B . 0.9900 ?
C14 C20 . 1.534(6) ?
C14 C15 . 1.537(6) ?
C14 H14 . 1.0000 ?
C15 C16 . 1.535(6) ?
C15 H15A . 0.9900 ?
C15 H15B . 0.9900 ?
C16 C17 . 1.541(6) ?
C16 C18 . 1.542(6) ?
C16 H16 . 1.0000 ?
C17 H17A . 0.9900 ?
C17 H17B . 0.9900 ?
C18 C19 . 1.535(6) ?
C18 H18A . 0.9900 ?
C18 H18B . 0.9900 ?
C19 C20 . 1.541(6) ?
C19 C21 . 1.543(5) ?
C19 H19 . 1.0000 ?
C20 H20A . 0.9900 ?
C20 H20B . 0.9900 ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C22 O1 2_556 1.263(5) ?
C22 C23 . 1.512(6) ?
C23 H23A . 0.9800 ?
C23 H23B . 0.9800 ?
C23 H23C . 0.9800 ?
C24 O2 2_556 1.268(5) ?
C24 C25 . 1.510(6) ?
C25 H25A . 0.9800 ?
C25 H25B . 0.9800 ?
C25 H25C . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1 O5 0.83(5) 1.90(5) 2.555(5) 135(5)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139073192
