#------------------------------------------------------------------------------
#$Date: 2016-02-18 16:37:37 +0100 (jue 18 de feb de 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/51/1515168.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_1515168
loop_
_publ_author_name
'Siu, Fung-Ming'
'Lin, Iris Wing-Shan'
'Yan, Kun'
'Lok, Chun-Nam'
'Low, Kam-Hung'
'Leung, Thomas Yun-Chung'
'Lam, Tin-Lun'
'Che, Chi-Ming'
_publ_section_title
;
 Anticancer dirhodium(ii,ii) carboxylates as potent inhibitors of
 ubiquitin-proteasome system
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              1785
_journal_paper_doi               10.1039/c2sc00620k
_journal_volume                  3
_journal_year                    2012
_chemical_formula_moiety         'C20 H30 N6 O4 Rh2, 2(H2 O)'
_chemical_formula_sum            'C20 H34 N6 O6 Rh2'
_chemical_formula_weight         660.35
_chemical_name_systematic
;
?
;
_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                 104.0390(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3720(4)
_cell_length_b                   8.7441(2)
_cell_length_c                   17.2355(5)
_cell_measurement_reflns_used    174
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      3
_cell_volume                     2393.71(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30491
_diffrn_reflns_theta_full        66.26
_diffrn_reflns_theta_max         66.26
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    11.577
_exptl_absorpt_correction_T_max  0.629
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.922
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4091
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0300
_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)+(0.0462P)²+5.0305P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                3864
_reflns_number_total             4091
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2sc00620k.txt
_cod_data_source_block           iris3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1515168
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 0.988968(14) 0.98936(3) 0.067621(14) 0.01547(11) Uani 1 1 d .
Rh2 Rh 0.523401(17) -0.00486(3) 0.073248(15) 0.02338(12) Uani 1 1 d .
N1 N 1.10476(16) 0.9003(3) 0.09720(15) 0.0189(6) Uani 1 1 d .
N2 N 0.96374(16) 0.7981(3) -0.08350(15) 0.0193(6) Uani 1 1 d .
N3 N 0.41189(18) 0.0914(3) 0.07211(16) 0.0243(6) Uani 1 1 d .
N4 N 0.46968(17) -0.2132(3) 0.06310(16) 0.0226(6) Uani 1 1 d .
N5 N 0.9563(2) 0.9610(4) 0.18532(18) 0.0304(7) Uani 1 1 d .
N6 N 0.5713(2) -0.0057(4) 0.2060(2) 0.0334(8) Uani 1 1 d .
O1 O 1.13049(13) 0.9156(3) -0.02755(13) 0.0242(5) Uani 1 1 d .
O2 O 0.94066(14) 0.7698(3) 0.04200(12) 0.0215(5) Uani 1 1 d .
O3 O 0.36314(15) 0.1002(3) -0.06436(14) 0.0347(6) Uani 1 1 d .
O4 O 0.42271(18) -0.2099(3) -0.07361(14) 0.0403(7) Uani 1 1 d .
O5 O 1.22936(18) 0.8159(4) -0.13400(17) 0.0428(7) Uani 1 1 d D
H51 H 1.194(2) 0.863(5) -0.103(3) 0.064 Uiso 1 1 d D
H52 H 1.2840(15) 0.860(5) -0.114(3) 0.064 Uiso 1 1 d D
O6 O 0.3056(4) 0.2999(8) -0.1883(3) 0.123(2) Uani 1 1 d D
H61 H 0.328(6) 0.232(9) -0.142(3) 0.184 Uiso 1 1 d D
H62 H 0.328(6) 0.265(11) -0.234(3) 0.184 Uiso 1 1 d D
C1 C 1.15056(19) 0.8775(4) 0.04656(19) 0.0208(7) Uani 1 1 d .
C2 C 1.2319(2) 0.7950(4) 0.0828(2) 0.0272(8) Uani 1 1 d .
H2A H 1.2808 0.8520 0.0734 0.033 Uiso 1 1 calc R
H2B H 1.2317 0.6907 0.0604 0.033 Uiso 1 1 calc R
C3 C 1.2340(2) 0.7894(5) 0.1720(2) 0.0349(9) Uani 1 1 d .
H3A H 1.2783 0.8576 0.2028 0.042 Uiso 1 1 calc R
H3B H 1.2447 0.6839 0.1929 0.042 Uiso 1 1 calc R
C4 C 1.1462(2) 0.8442(4) 0.17706(19) 0.0255(7) Uani 1 1 d .
H4A H 1.1137 0.7589 0.1926 0.031 Uiso 1 1 calc R
H4B H 1.1510 0.9271 0.2171 0.031 Uiso 1 1 calc R
C5 C 0.93716(18) 0.7232(4) -0.02897(18) 0.0188(6) Uani 1 1 d .
C6 C 0.8990(2) 0.5700(4) -0.0590(2) 0.0247(7) Uani 1 1 d .
H6A H 0.8373 0.5700 -0.0649 0.030 Uiso 1 1 calc R
H6B H 0.9245 0.4863 -0.0224 0.030 Uiso 1 1 calc R
C7 C 0.9203(3) 0.5539(4) -0.1397(2) 0.0333(8) Uani 1 1 d .
H7A H 0.8708 0.5181 -0.1809 0.040 Uiso 1 1 calc R
H7B H 0.9672 0.4807 -0.1365 0.040 Uiso 1 1 calc R
C8 C 0.9463(3) 0.7159(4) -0.1594(2) 0.0305(8) Uani 1 1 d .
H8A H 0.9971 0.7122 -0.1810 0.037 Uiso 1 1 calc R
H8B H 0.9002 0.7660 -0.1992 0.037 Uiso 1 1 calc R
C9 C 0.3562(2) 0.1274(4) 0.00680(19) 0.0252(7) Uani 1 1 d .
C10 C 0.2807(2) 0.2082(4) 0.0224(2) 0.0275(8) Uani 1 1 d .
H10A H 0.2278 0.1569 -0.0055 0.033 Uiso 1 1 calc R
H10B H 0.2788 0.3163 0.0049 0.033 Uiso 1 1 calc R
C11 C 0.2942(2) 0.1969(4) 0.1143(2) 0.0283(8) Uani 1 1 d .
H11A H 0.2871 0.2980 0.1376 0.034 Uiso 1 1 calc R
H11B H 0.2541 0.1237 0.1286 0.034 Uiso 1 1 calc R
C12 C 0.3855(2) 0.1396(4) 0.14349(19) 0.0279(8) Uani 1 1 d .
H12A H 0.4223 0.2225 0.1714 0.034 Uiso 1 1 calc R
H12B H 0.3882 0.0527 0.1808 0.034 Uiso 1 1 calc R
C13 C 0.4307(2) -0.2722(4) -0.0050(2) 0.0273(8) Uani 1 1 d .
C14 C 0.3917(2) -0.4251(4) 0.0033(2) 0.0300(8) Uani 1 1 d .
H14A H 0.4119 -0.5041 -0.0287 0.036 Uiso 1 1 calc R
H14B H 0.3295 -0.4198 -0.0137 0.036 Uiso 1 1 calc R
C15 C 0.4212(3) -0.4584(5) 0.0922(2) 0.0327(8) Uani 1 1 d .
H15A H 0.4624 -0.5434 0.1020 0.039 Uiso 1 1 calc R
H15B H 0.3731 -0.4860 0.1147 0.039 Uiso 1 1 calc R
C16 C 0.4626(2) -0.3087(4) 0.1296(2) 0.0296(8) Uani 1 1 d .
H16A H 0.4273 -0.2585 0.1613 0.036 Uiso 1 1 calc R
H16B H 0.5189 -0.3294 0.1649 0.036 Uiso 1 1 calc R
C17 C 0.6053(3) 0.0082(5) 0.2714(2) 0.0374(11) Uani 1 1 d .
C18 C 0.6490(3) 0.0270(7) 0.3556(3) 0.0553(14) Uani 1 1 d .
H18A H 0.6197 0.1039 0.3802 0.083 Uiso 1 1 calc R
H18B H 0.7070 0.0605 0.3595 0.083 Uiso 1 1 calc R
H18C H 0.6496 -0.0708 0.3835 0.083 Uiso 1 1 calc R
C19 C 0.9107(3) 0.9358(6) 0.2224(3) 0.0515(12) Uani 1 1 d .
C20 C 0.8505(5) 0.9039(12) 0.2692(4) 0.126(4) Uani 1 1 d .
H20A H 0.8017 0.8509 0.2359 0.189 Uiso 1 1 calc R
H20B H 0.8322 1.0002 0.2887 0.189 Uiso 1 1 calc R
H20C H 0.8768 0.8391 0.3148 0.189 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh 0.0927 3.6045 '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
N1 Rh1 N2 90.87(11) . 3_775
N1 Rh1 O2 89.02(10) . .
N2 Rh1 O2 175.56(9) 3_775 .
N1 Rh1 O1 175.42(9) . 3_775
N2 Rh1 O1 88.61(10) 3_775 3_775
O2 Rh1 O1 91.14(9) . 3_775
N1 Rh1 N5 98.43(11) . .
N2 Rh1 N5 98.54(11) 3_775 .
O2 Rh1 N5 85.86(10) . .
O1 Rh1 N5 86.15(10) 3_775 .
N1 Rh1 Rh1 85.56(7) . 3_775
N2 Rh1 Rh1 85.32(7) 3_775 3_775
O2 Rh1 Rh1 90.25(6) . 3_775
O1 Rh1 Rh1 89.86(6) 3_775 3_775
N5 Rh1 Rh1 174.36(9) . 3_775
N3 Rh2 N4 90.09(11) . .
N3 Rh2 O4 90.31(12) . 3_655
N4 Rh2 O4 175.31(10) . 3_655
N3 Rh2 O3 175.23(10) . 3_655
N4 Rh2 O3 90.58(11) . 3_655
O4 Rh2 O3 88.64(12) 3_655 3_655
N3 Rh2 N6 95.96(12) . .
N4 Rh2 N6 97.11(11) . .
O4 Rh2 N6 87.50(10) 3_655 .
O3 Rh2 N6 88.64(11) 3_655 .
N3 Rh2 Rh2 85.37(8) . 3_655
N4 Rh2 Rh2 85.48(8) . 3_655
O4 Rh2 Rh2 89.89(7) 3_655 3_655
O3 Rh2 Rh2 89.98(6) 3_655 3_655
N6 Rh2 Rh2 177.08(9) . 3_655
C1 N1 C4 111.7(3) . .
C1 N1 Rh1 123.8(2) . .
C4 N1 Rh1 124.4(2) . .
C5 N2 C8 111.9(3) . .
C5 N2 Rh1 123.5(2) . 3_775
C8 N2 Rh1 124.3(2) . 3_775
C9 N3 C12 111.7(3) . .
C9 N3 Rh2 123.7(2) . .
C12 N3 Rh2 124.6(2) . .
C13 N4 C16 111.7(3) . .
C13 N4 Rh2 123.1(2) . .
C16 N4 Rh2 124.9(2) . .
C19 N5 Rh1 152.0(3) . .
C17 N6 Rh2 169.3(3) . .
C1 O1 Rh1 115.26(19) . 3_775
C5 O2 Rh1 115.1(2) . .
C9 O3 Rh2 115.7(2) . 3_655
C13 O4 Rh2 115.8(2) . 3_655
O1 C1 N1 125.4(3) . .
O1 C1 C2 121.5(3) . .
N1 C1 C2 113.0(3) . .
C1 C2 C3 103.5(3) . .
C2 C3 C4 104.7(3) . .
N1 C4 C3 106.1(3) . .
O2 C5 N2 125.8(3) . .
O2 C5 C6 121.9(3) . .
N2 C5 C6 112.3(3) . .
C5 C6 C7 103.1(3) . .
C6 C7 C8 104.7(3) . .
N2 C8 C7 105.1(3) . .
O3 C9 N3 125.1(3) . .
O3 C9 C10 121.8(3) . .
N3 C9 C10 113.1(3) . .
C9 C10 C11 103.5(3) . .
C12 C11 C10 104.0(3) . .
N3 C12 C11 106.3(3) . .
O4 C13 N4 125.7(3) . .
O4 C13 C14 121.1(3) . .
N4 C13 C14 113.2(3) . .
C13 C14 C15 103.1(3) . .
C14 C15 C16 105.1(3) . .
N4 C16 C15 105.7(3) . .
N6 C17 C18 179.7(5) . .
N5 C19 C20 179.0(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 1.998(3) .
Rh1 N2 2.006(3) 3_775
Rh1 O2 2.082(2) .
Rh1 O1 2.083(2) 3_775
Rh1 N5 2.234(3) .
Rh1 Rh1 2.4509(5) 3_775
Rh2 N3 2.006(3) .
Rh2 N4 2.012(3) .
Rh2 O4 2.074(3) 3_655
Rh2 O3 2.075(3) 3_655
Rh2 N6 2.231(3) .
Rh2 Rh2 2.4558(5) 3_655
N1 C1 1.297(4) .
N1 C4 1.464(4) .
N2 C5 1.304(4) .
N2 C8 1.458(4) .
N2 Rh1 2.006(3) 3_775
N3 C9 1.304(4) .
N3 C12 1.462(4) .
N4 C13 1.300(4) .
N4 C16 1.445(4) .
N5 C19 1.115(6) .
N6 C17 1.136(5) .
O1 C1 1.283(4) .
O1 Rh1 2.083(2) 3_775
O2 C5 1.277(4) .
O3 C9 1.281(4) .
O3 Rh2 2.075(3) 3_655
O4 C13 1.279(4) .
O4 Rh2 2.074(3) 3_655
C1 C2 1.509(4) .
C2 C3 1.529(5) .
C3 C4 1.537(5) .
C5 C6 1.516(5) .
C6 C7 1.521(5) .
C7 C8 1.540(5) .
C9 C10 1.504(5) .
C10 C11 1.547(5) .
C11 C12 1.540(5) .
C13 C14 1.503(5) .
C14 C15 1.519(5) .
C15 C16 1.541(5) .
C17 C18 1.463(6) .
C19 C20 1.444(7) .
