#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:20:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178895 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/24/4112458.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_4112458
loop_
_publ_author_name
'Scott A. Hilderbrand'
'Mi Hee Lim'
'Stephen J. Lippard'
_publ_section_title
;
 Dirhodium Tetracarboxylate Scaffolds as Reversible Fluorescence-Based
 Nitric Oxide Sensors
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4972
_journal_page_last               4978
_journal_paper_doi               10.1021/ja038471j
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C16 H28 N2 O10 Rh2'
_chemical_formula_weight         614.22
_chemical_name_systematic
; 
 ? 
;
_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                105.432(14)
_cell_angle_beta                 106.84(2)
_cell_angle_gamma                96.004(18)
_cell_formula_units_Z            2
_cell_length_a                   8.440(3)
_cell_length_b                   10.463(3)
_cell_length_c                   14.299(4)
_cell_measurement_temperature    173(2)
_cell_volume                     1142.2(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10171
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    1.496
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.847472
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            Burgundy
_exptl_crystal_density_diffrn    1.786
_exptl_crystal_density_meas      0
_exptl_crystal_description       Needle
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     275
_refine_ls_number_reflns         5173
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0342
_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)+(0.0311P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                4000
_reflns_number_total             5173
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja038471jsi20040128_120252.cif
_cod_data_source_block           Complex10
_cod_database_code               4112458
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.47274(3) 0.61420(3) 1.04038(2) 0.02250(8) Uani 1 1 d .
O4 O 0.5302(3) 0.6690(2) 0.92602(17) 0.0275(5) Uani 1 1 d .
O3 O 0.4196(3) 0.5357(2) 1.14633(17) 0.0270(5) Uani 1 1 d .
O2 O 0.7226(3) 0.6593(2) 1.12498(17) 0.0282(5) Uani 1 1 d .
O1 O 0.2270(3) 0.5444(2) 0.94915(18) 0.0297(6) Uani 1 1 d .
N1 N 0.4471(4) 0.7940(3) 1.1095(2) 0.0312(7) Uani 1 1 d .
C1 C 0.8183(4) 0.5755(4) 1.1118(3) 0.0286(8) Uani 1 1 d .
C2 C 0.5695(4) 0.5859(4) 0.8580(3) 0.0255(7) Uani 1 1 d .
O5 O 0.5013(4) 0.8424(3) 1.1958(2) 0.0517(8) Uani 1 1 d .
C3 C 1.0031(4) 0.6207(4) 1.1747(3) 0.0335(9) Uani 1 1 d .
H3A H 1.0682 0.5629 1.1400 0.040 Uiso 1 1 calc R
H3B H 1.0204 0.6078 1.2428 0.040 Uiso 1 1 calc R
C4 C 0.6049(5) 0.6344(4) 0.7751(3) 0.0313(8) Uani 1 1 d .
H4A H 0.5036 0.6002 0.7127 0.038 Uiso 1 1 calc R
H4B H 0.6981 0.5942 0.7583 0.038 Uiso 1 1 calc R
C5 C 0.6518(5) 0.7863(4) 0.8010(3) 0.0361(9) Uani 1 1 d .
H5A H 0.7606 0.8204 0.8582 0.043 Uiso 1 1 calc R
H5B H 0.5647 0.8284 0.8245 0.043 Uiso 1 1 calc R
C6 C 1.0537(5) 0.7951(4) 1.0885(3) 0.0450(10) Uani 1 1 d .
H6A H 1.1057 0.7316 1.0488 0.067 Uiso 1 1 calc R
H6B H 1.1102 0.8880 1.1017 0.067 Uiso 1 1 calc R
H6C H 0.9338 0.7828 1.0495 0.067 Uiso 1 1 calc R
C7 C 1.0716(5) 0.7686(4) 1.1900(3) 0.0384(9) Uani 1 1 d .
H7A H 1.0097 0.8269 1.2270 0.046 Uiso 1 1 calc R
H7B H 1.1923 0.7927 1.2330 0.046 Uiso 1 1 calc R
C8 C 0.6674(5) 0.8281(4) 0.7095(3) 0.0403(10) Uani 1 1 d .
H8A H 0.7442 0.7788 0.6812 0.060 Uiso 1 1 calc R
H8B H 0.7120 0.9255 0.7318 0.060 Uiso 1 1 calc R
H8C H 0.5559 0.8067 0.6566 0.060 Uiso 1 1 calc R
Rh2 Rh 0.86353(3) 0.44819(3) 0.50643(2) 0.02550(8) Uani 1 1 d .
O6 O 0.7562(3) 0.5890(2) 0.44927(19) 0.0331(6) Uani 1 1 d .
O9 O 0.8109(3) 0.3249(2) 0.36017(18) 0.0319(6) Uani 1 1 d .
O7 O 0.9978(3) 0.3184(2) 0.56185(18) 0.0322(6) Uani 1 1 d .
N2 N 0.6613(4) 0.3712(3) 0.5290(2) 0.0374(8) Uani 1 1 d .
O10 O 0.6694(4) 0.3492(3) 0.6044(2) 0.0525(8) Uani 1 1 d .
C9 C 1.1541(5) 0.3251(4) 0.5716(3) 0.0302(8) Uani 1 1 d .
C13 C 1.2389(5) 0.2194(4) 0.6083(3) 0.0393(10) Uani 1 1 d .
H13A H 1.1806 0.1855 0.6504 0.047 Uiso 1 1 calc R
H13B H 1.3576 0.2600 0.6519 0.047 Uiso 1 1 calc R
C14 C 1.2340(7) 0.1016(4) 0.5159(3) 0.0562(13) Uani 1 1 d .
H14A H 1.1153 0.0644 0.4711 0.067 Uiso 1 1 calc R
H14B H 1.2955 0.1359 0.4753 0.067 Uiso 1 1 calc R
C16 C 1.3121(7) -0.0101(5) 0.5484(4) 0.0703(15) Uani 1 1 d .
H16A H 1.4308 0.0256 0.5908 0.105 Uiso 1 1 calc R
H16B H 1.3049 -0.0835 0.4872 0.105 Uiso 1 1 calc R
H16C H 1.2511 -0.0448 0.5881 0.105 Uiso 1 1 calc R
O8 O 0.9442(3) 0.5808(2) 0.65096(17) 0.0292(6) Uani 1 1 d .
C10 C 0.8659(5) 0.2478(3) 0.2036(3) 0.0308(8) Uani 1 1 d .
H10A H 0.9636 0.2582 0.1793 0.037 Uiso 1 1 calc R
H10B H 0.7732 0.2788 0.1603 0.037 Uiso 1 1 calc R
C11 C 0.8097(5) 0.0999(4) 0.1884(3) 0.0385(9) Uani 1 1 d .
H11A H 0.7160 0.0886 0.2159 0.046 Uiso 1 1 calc R
H11B H 0.9045 0.0659 0.2270 0.046 Uiso 1 1 calc R
C12 C 0.9146(4) 0.3371(3) 0.3125(3) 0.0281(8) Uani 1 1 d .
C15 C 0.7521(5) 0.0184(4) 0.0760(3) 0.0473(11) Uani 1 1 d .
H15A H 0.6632 0.0557 0.0371 0.071 Uiso 1 1 calc R
H15B H 0.7078 -0.0759 0.0676 0.071 Uiso 1 1 calc R
H15C H 0.8477 0.0224 0.0504 0.071 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Rh1 O4 94.35(11) . .
N1 Rh1 O2 90.52(11) . .
O4 Rh1 O2 89.81(10) . .
N1 Rh1 O1 96.74(11) . .
O4 Rh1 O1 90.67(10) . .
O2 Rh1 O1 172.67(9) . .
N1 Rh1 O3 92.88(11) . .
O4 Rh1 O3 172.77(9) . .
O2 Rh1 O3 89.89(10) . .
O1 Rh1 O3 88.72(10) . .
N1 Rh1 Rh1 175.91(9) . 2_667
O4 Rh1 Rh1 86.05(7) . 2_667
O2 Rh1 Rh1 85.42(7) . 2_667
O1 Rh1 Rh1 87.32(7) . 2_667
O3 Rh1 Rh1 86.72(7) . 2_667
C2 O4 Rh1 121.3(2) . .
C2 O3 Rh1 120.3(2) 2_667 .
C1 O2 Rh1 121.7(2) . .
C1 O1 Rh1 119.5(2) 2_667 .
O5 N1 Rh1 122.7(3) . .
O2 C1 O1 126.0(3) . 2_667
O2 C1 C3 117.7(3) . .
O1 C1 C3 116.3(3) 2_667 .
O4 C2 O3 125.6(3) . 2_667
O4 C2 C4 117.4(3) . .
O3 C2 C4 117.0(3) 2_667 .
C1 C3 C7 113.0(3) . .
C2 C4 C5 115.4(3) . .
C4 C5 C8 112.2(3) . .
C6 C7 C3 111.9(3) . .
N2 Rh2 O8 90.39(12) . .
N2 Rh2 O7 92.31(12) . .
O8 Rh2 O7 88.93(10) . .
N2 Rh2 O9 96.83(12) . .
O8 Rh2 O9 172.76(9) . .
O7 Rh2 O9 90.21(10) . .
N2 Rh2 O6 94.86(12) . .
O8 Rh2 O6 90.57(10) . .
O7 Rh2 O6 172.82(10) . .
O9 Rh2 O6 89.40(10) . .
N2 Rh2 Rh2 175.14(10) . 2_766
O8 Rh2 Rh2 85.40(7) . 2_766
O7 Rh2 Rh2 85.19(7) . 2_766
O9 Rh2 Rh2 87.36(7) . 2_766
O6 Rh2 Rh2 87.63(7) . 2_766
C9 O6 Rh2 119.4(2) 2_766 .
C12 O9 Rh2 119.5(2) . .
C9 O7 Rh2 122.0(2) . .
O10 N2 Rh2 121.1(3) . .
O6 C9 O7 125.8(3) 2_766 .
O6 C9 C13 116.6(3) 2_766 .
O7 C9 C13 117.6(3) . .
C9 C13 C14 110.0(3) . .
C16 C14 C13 112.2(4) . .
C12 O8 Rh2 122.0(2) 2_766 .
C12 C10 C11 114.4(3) . .
C10 C11 C15 111.1(3) . .
O9 C12 O8 125.7(3) . 2_766
O9 C12 C10 117.2(3) . .
O8 C12 C10 117.1(3) 2_766 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 1.945(3) .
Rh1 O4 2.034(2) .
Rh1 O2 2.035(2) .
Rh1 O1 2.036(2) .
Rh1 O3 2.037(2) .
Rh1 Rh1 2.5151(8) 2_667
O4 C2 1.268(4) .
O3 C2 1.272(4) 2_667
O2 C1 1.267(4) .
O1 C1 1.267(4) 2_667
N1 O5 1.131(4) .
C1 O1 1.267(4) 2_667
C1 C3 1.507(5) .
C2 O3 1.272(4) 2_667
C2 C4 1.499(5) .
C3 C7 1.528(5) .
C4 C5 1.513(5) .
C5 C8 1.519(5) .
C6 C7 1.517(5) .
Rh2 N2 1.958(3) .
Rh2 O8 2.030(2) .
Rh2 O7 2.032(2) .
Rh2 O9 2.035(2) .
Rh2 O6 2.037(2) .
Rh2 Rh2 2.5191(9) 2_766
O6 C9 1.266(4) 2_766
O9 C12 1.271(4) .
O7 C9 1.278(4) .
N2 O10 1.146(4) .
C9 O6 1.266(4) 2_766
C9 C13 1.506(5) .
C13 C14 1.536(6) .
C14 C16 1.514(6) .
O8 C12 1.271(4) 2_766
C10 C12 1.497(5) .
C10 C11 1.508(5) .
C11 C15 1.508(5) .
C12 O8 1.271(4) 2_766
