#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/89/4328993.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4328993
loop_
_publ_author_name
'D. Krishna Kumar'
'Alexander S. Filatov'
'Margaret Napier'
'Jinyu Sun'
'Evgeny V. Dikarev'
'Marina A. Petrukhina'
_publ_contact_author_address
;
Department of Chemistry
University at Albany
1400 Washington ave
Albany NY 12222
USA
;
_publ_contact_author_email       mpetrukhina@albany.edu
_publ_contact_author_fax         518-442-3462
_publ_contact_author_name
;
Petrukhina, Marina 
;
_publ_contact_author_phone       518-442-4406
_publ_section_title
;
 Dirhodium Paddlewheel with Functionalized Carboxylate Bridges: New
 Building Block for Self-Assembly and Immobilization on Solid Support
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4855
_journal_page_last               4861
_journal_paper_doi               10.1021/ic300382j
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C46 H48 O18 Rh2, C6 H14'
_chemical_formula_sum            'C52 H62 O18 Rh2'
_chemical_formula_weight         1180.84
_chemical_name_systematic
; 
 tetra-(4-ethoxycarbonyl benzoate)-
 bis-acetone- dirhodium (II,II),hexane solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.940(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.8635(13)
_cell_length_b                   13.1392(17)
_cell_length_c                   20.333(3)
_cell_measurement_reflns_used    7804
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.38
_cell_measurement_theta_min      28.27
_cell_volume                     2625.3(6)
_computing_cell_refinement       'SAINT Ver. 6.22  (Bruker-AXS, 2003)'
_computing_data_collection       'SMART Ver. 5.622 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT Ver. 6.22'
_computing_molecular_graphics    'SHELXTL Ver. 6.14'
_computing_publication_material  'SHELXTL Ver. 6.14'
_computing_structure_refinement  'SHELXTL Ver. 6.14'
_computing_structure_solution    'SHELXTL Ver. 6.14 (Bruker-AXS, 2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '0.30° ω scans'
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19722
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.9725
_exptl_absorpt_correction_T_min  0.8725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       needle
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         5151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0432P)²+1.6725P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                4719
_reflns_number_total             5151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300382j_si_002_2.cif
_cod_data_source_block           {[Rh2(C10H9O4)4(C3H6O)2](C6H14)}
_cod_original_cell_volume        2625.4(6)
_cod_database_code               4328993
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 1.057012(14) 0.464813(11) 0.455766(7) 0.01830(7) Uani 1 1 d .
O1 O 0.88204(14) 0.38978(11) 0.42693(7) 0.0230(3) Uani 1 1 d .
O2 O 1.11509(14) 0.34580(11) 0.51642(7) 0.0226(3) Uani 1 1 d .
O3 O 1.22697(14) 0.54270(10) 0.48993(7) 0.0227(3) Uani 1 1 d .
O4 O 0.99562(14) 0.58715(11) 0.40085(7) 0.0235(3) Uani 1 1 d .
O5 O 1.16994(15) 0.41119(11) 0.36911(7) 0.0260(3) Uani 1 1 d .
O7 O 0.28490(18) 0.14301(15) 0.30993(8) 0.0436(5) Uani 1 1 d .
O8 O 0.20071(14) 0.17464(12) 0.40671(7) 0.0272(3) Uani 1 1 d .
O9 O 1.24239(19) -0.08836(13) 0.71525(9) 0.0404(4) Uani 1 1 d .
O10 O 1.10164(19) -0.01793(14) 0.78307(10) 0.0433(5) Uani 1 1 d .
C1 C 0.77907(19) 0.40064(15) 0.45980(10) 0.0204(4) Uani 1 1 d .
C2 C 1.0733(2) 0.34377(16) 0.57381(10) 0.0216(4) Uani 1 1 d .
C3 C 1.1409(2) 0.41394(16) 0.31007(11) 0.0270(5) Uani 1 1 d .
C4 C 0.6543(2) 0.34118(15) 0.43686(10) 0.0204(4) Uani 1 1 d .
C5 C 0.5345(2) 0.35414(16) 0.46753(10) 0.0224(4) Uani 1 1 d .
H5 H 0.5322 0.4004 0.5033 0.027 Uiso 1 1 calc R
C6 C 0.4187(2) 0.29984(16) 0.44603(10) 0.0229(4) Uani 1 1 d .
H6 H 0.3371 0.3087 0.4671 0.028 Uiso 1 1 calc R
C7 C 0.4223(2) 0.23229(16) 0.39346(10) 0.0227(4) Uani 1 1 d .
C8 C 0.5425(2) 0.21846(17) 0.36330(10) 0.0255(4) Uani 1 1 d .
H8 H 0.5450 0.1718 0.3277 0.031 Uiso 1 1 calc R
C9 C 0.6582(2) 0.27237(16) 0.38495(10) 0.0243(4) Uani 1 1 d .
H9 H 0.7402 0.2625 0.3645 0.029 Uiso 1 1 calc R
C10 C 0.2980(2) 0.17790(16) 0.36507(11) 0.0268(5) Uani 1 1 d .
C11 C 0.0698(2) 0.13428(19) 0.38047(12) 0.0329(5) Uani 1 1 d .
H11A H 0.0815 0.0659 0.3614 0.039 Uiso 1 1 calc R
H11B H 0.0281 0.1795 0.3454 0.039 Uiso 1 1 calc R
C12 C -0.0187(2) 0.12833(18) 0.43654(12) 0.0341(5) Uani 1 1 d .
H12A H 0.0220 0.0814 0.4701 0.051 Uiso 1 1 calc R
H12B H -0.1091 0.1036 0.4202 0.051 Uiso 1 1 calc R
H12C H -0.0269 0.1961 0.4560 0.051 Uiso 1 1 calc R
C13 C 1.1063(2) 0.25193(16) 0.61539(10) 0.0220(4) Uani 1 1 d .
C14 C 1.0523(2) 0.24363(17) 0.67639(11) 0.0268(5) Uani 1 1 d .
H14 H 0.9991 0.2974 0.6918 0.032 Uiso 1 1 calc R
C15 C 1.0761(2) 0.15750(17) 0.71422(11) 0.0271(5) Uani 1 1 d .
H15 H 1.0384 0.1519 0.7555 0.033 Uiso 1 1 calc R
C16 C 1.1548(2) 0.07872(16) 0.69233(10) 0.0243(4) Uani 1 1 d .
C17 C 1.2136(2) 0.08868(17) 0.63272(11) 0.0259(4) Uani 1 1 d .
H17 H 1.2709 0.0364 0.6186 0.031 Uiso 1 1 calc R
C18 C 1.1887(2) 0.17470(16) 0.59409(10) 0.0247(4) Uani 1 1 d .
H18 H 1.2278 0.1809 0.5532 0.030 Uiso 1 1 calc R
C19 C 1.1738(2) -0.01830(17) 0.73068(12) 0.0276(5) Uani 1 1 d .
C20 C 1.1046(3) -0.1082(2) 0.82490(16) 0.0528(8) Uani 1 1 d .
H20A H 1.1651 -0.0968 0.8656 0.063 Uiso 1 1 calc R
H20B H 1.1393 -0.1673 0.8012 0.063 Uiso 1 1 calc R
C21 C 0.9628(4) -0.1280(3) 0.84167(17) 0.0620(9) Uani 1 1 d .
H21A H 0.9281 -0.0679 0.8634 0.093 Uiso 1 1 calc R
H21B H 0.9623 -0.1865 0.8715 0.093 Uiso 1 1 calc R
H21C H 0.9048 -0.1425 0.8012 0.093 Uiso 1 1 calc R
C22 C 0.9974(3) 0.4269(2) 0.28014(12) 0.0440(6) Uani 1 1 d .
H22A H 0.9343 0.4181 0.3144 0.066 Uiso 1 1 calc R
H22B H 0.9779 0.3759 0.2454 0.066 Uiso 1 1 calc R
H22C H 0.9864 0.4952 0.2611 0.066 Uiso 1 1 calc R
C23 C 1.2482(3) 0.4030(2) 0.26316(12) 0.0408(6) Uani 1 1 d .
H23A H 1.3381 0.4041 0.2877 0.061 Uiso 1 1 calc R
H23B H 1.2412 0.4594 0.2315 0.061 Uiso 1 1 calc R
H23C H 1.2357 0.3383 0.2394 0.061 Uiso 1 1 calc R
C24 C 0.7621(3) 0.6377(3) 0.92686(15) 0.0624(9) Uani 1 1 d .
H24A H 0.6935 0.5839 0.9198 0.094 Uiso 1 1 calc R
H24B H 0.7547 0.6844 0.8892 0.094 Uiso 1 1 calc R
H24C H 0.7470 0.6752 0.9672 0.094 Uiso 1 1 calc R
C25 C 0.9050(3) 0.5897(2) 0.93377(14) 0.0527(7) Uani 1 1 d .
H25A H 0.9175 0.5486 0.8939 0.063 Uiso 1 1 calc R
H25B H 0.9740 0.6446 0.9362 0.063 Uiso 1 1 calc R
C26 C 0.9287(3) 0.5224(2) 0.99446(14) 0.0511(8) Uani 1 1 d .
H26A H 0.8622 0.4658 0.9906 0.061 Uiso 1 1 calc R
H26B H 0.9104 0.5629 1.0338 0.061 Uiso 1 1 calc R
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Rh1 O1 91.14(6) . .
O4 Rh1 O3 89.28(6) . .
O1 Rh1 O3 176.38(5) . .
O4 Rh1 O2 176.35(5) . .
O1 Rh1 O2 89.42(6) . .
O3 Rh1 O2 89.94(6) . .
O4 Rh1 O5 87.81(5) . .
O1 Rh1 O5 94.97(5) . .
O3 Rh1 O5 88.64(6) . .
O2 Rh1 O5 95.74(5) . .
O4 Rh1 Rh1 88.28(4) . 3_766
O1 Rh1 Rh1 87.81(4) . 3_766
O3 Rh1 Rh1 88.61(4) . 3_766
O2 Rh1 Rh1 88.13(4) . 3_766
O5 Rh1 Rh1 175.25(4) . 3_766
C1 O1 Rh1 119.45(13) . .
C2 O2 Rh1 118.30(13) . .
C1 O3 Rh1 118.38(13) 3_766 .
C2 O4 Rh1 119.35(13) 3_766 .
C3 O5 Rh1 131.99(14) . .
C10 O8 C11 116.31(17) . .
C19 O10 C20 118.6(2) . .
O3 C1 O1 125.73(18) 3_766 .
O3 C1 C4 117.52(17) 3_766 .
O1 C1 C4 116.75(17) . .
O4 C2 O2 125.80(19) 3_766 .
O4 C2 C13 116.51(17) 3_766 .
O2 C2 C13 117.69(18) . .
O5 C3 C23 120.8(2) . .
O5 C3 C22 122.6(2) . .
C23 C3 C22 116.6(2) . .
C9 C4 C5 119.90(19) . .
C9 C4 C1 119.91(18) . .
C5 C4 C1 120.18(18) . .
C6 C5 C4 120.26(19) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 119.70(19) . .
C5 C6 H6 120.2 . .
C7 C6 H6 120.2 . .
C8 C7 C6 120.04(19) . .
C8 C7 C10 118.01(19) . .
C6 C7 C10 121.84(19) . .
C9 C8 C7 120.23(19) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C8 C9 C4 119.85(19) . .
C8 C9 H9 120.1 . .
C4 C9 H9 120.1 . .
O7 C10 O8 123.5(2) . .
O7 C10 C7 124.0(2) . .
O8 C10 C7 112.46(18) . .
O8 C11 C12 107.30(18) . .
O8 C11 H11A 110.3 . .
C12 C11 H11A 110.3 . .
O8 C11 H11B 110.3 . .
C12 C11 H11B 110.3 . .
H11A C11 H11B 108.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C18 C13 C14 119.8(2) . .
C18 C13 C2 121.17(18) . .
C14 C13 C2 119.02(18) . .
C15 C14 C13 120.1(2) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 120.4(2) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C15 C16 C17 119.6(2) . .
C15 C16 C19 121.03(19) . .
C17 C16 C19 119.3(2) . .
C18 C17 C16 120.2(2) . .
C18 C17 H17 119.9 . .
C16 C17 H17 119.9 . .
C17 C18 C13 119.86(19) . .
C17 C18 H18 120.1 . .
C13 C18 H18 120.1 . .
O9 C19 O10 124.4(2) . .
O9 C19 C16 124.4(2) . .
O10 C19 C16 111.22(19) . .
O10 C20 C21 107.7(2) . .
O10 C20 H20A 110.2 . .
C21 C20 H20A 110.2 . .
O10 C20 H20B 110.2 . .
C21 C20 H20B 110.2 . .
H20A C20 H20B 108.5 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C3 C22 H22A 109.5 . .
C3 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
C3 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C3 C23 H23A 109.5 . .
C3 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C3 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C25 C24 H24A 109.5 . .
C25 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
C25 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
C26 C25 C24 112.8(3) . .
C26 C25 H25A 109.0 . .
C24 C25 H25A 109.0 . .
C26 C25 H25B 109.0 . .
C24 C25 H25B 109.0 . .
H25A C25 H25B 107.8 . .
C25 C26 C26 114.8(3) . 3_767
C25 C26 H26A 108.6 . .
C26 C26 H26A 108.6 3_767 .
C25 C26 H26B 108.6 . .
C26 C26 H26B 108.6 3_767 .
H26A C26 H26B 107.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 O4 2.0201(15) .
Rh1 O1 2.0298(14) .
Rh1 O3 2.0346(14) .
Rh1 O2 2.0428(14) .
Rh1 O5 2.2760(14) .
Rh1 Rh1 2.3883(3) 3_766
O1 C1 1.271(2) .
O2 C2 1.271(2) .
O3 C1 1.270(2) 3_766
O4 C2 1.270(2) 3_766
O5 C3 1.210(3) .
O7 C10 1.208(3) .
O8 C10 1.334(3) .
O8 C11 1.454(2) .
O9 C19 1.200(3) .
O10 C19 1.331(3) .
O10 C20 1.458(3) .
C1 O3 1.270(2) 3_766
C1 C4 1.498(3) .
C2 O4 1.270(2) 3_766
C2 C13 1.493(3) .
C3 C23 1.491(3) .
C3 C22 1.502(3) .
C4 C9 1.393(3) .
C4 C5 1.394(3) .
C5 C6 1.385(3) .
C5 H5 0.9500 .
C6 C7 1.392(3) .
C6 H6 0.9500 .
C7 C8 1.393(3) .
C7 C10 1.492(3) .
C8 C9 1.383(3) .
C8 H8 0.9500 .
C9 H9 0.9500 .
C11 C12 1.497(3) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C18 1.392(3) .
C13 C14 1.396(3) .
C14 C15 1.377(3) .
C14 H14 0.9500 .
C15 C16 1.390(3) .
C15 H15 0.9500 .
C16 C17 1.394(3) .
C16 C19 1.498(3) .
C17 C18 1.386(3) .
C17 H17 0.9500 .
C18 H18 0.9500 .
C20 C21 1.490(4) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 H23A 0.9800 .
C23 H23B 0.9800 .
C23 H23C 0.9800 .
C24 C25 1.540(5) .
C24 H24A 0.9800 .
C24 H24B 0.9800 .
C24 H24C 0.9800 .
C25 C26 1.519(4) .
C25 H25A 0.9900 .
C25 H25B 0.9900 .
C26 C26 1.524(7) 3_767
C26 H26A 0.9900 .
C26 H26B 0.9900 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139137223
