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#$Date: 2016-03-23 15:15:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321671.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_4321671
loop_
_publ_author_name
'Hitoshi Miyasaka'
'Cristian S. Campos-Fernández'
'José Ramón Galán-Mascarós'
'Kim R. Dunbar'
_publ_section_title
;
 One-Dimensional Assemblies of Dirhodium Units Bridged by
 N,N'-Dicyanoquinonediimine Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5870
_journal_page_last               5873
_journal_paper_doi               10.1021/ic0007097
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C24 H14 F12 N4 O8 Rh2'
_chemical_formula_weight         920.21
_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                67.555(5)
_cell_angle_beta                 88.810(5)
_cell_angle_gamma                63.899(5)
_cell_formula_units_Z            1
_cell_length_a                   8.570(5)
_cell_length_b                   9.135(5)
_cell_length_c                   11.871(5)
_cell_measurement_temperature    100(2)
_cell_volume                     759.1(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_sigmaI/netI    0.1349
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9118
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.215
_exptl_crystal_density_diffrn    2.013
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             448
_refine_diff_density_max         1.774
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.293
_refine_ls_extinction_coef       0.031(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          7.297
_refine_ls_shift/su_mean         0.518
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0823P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1646
_reflns_number_gt                2117
_reflns_number_total             3622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0007097_1.cif
_cod_data_source_block           '[Rh2(CF3CO2)4(DMDCNQI)]'
_cod_database_code               4321671
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.48254(8) 0.48683(9) -0.09571(5) 0.0215(2) Uani 1 1 d . . .
O1 O 0.2168(7) 0.6022(7) -0.0990(5) 0.0274(12) Uani 1 1 d . . .
O2 O 0.2493(7) 0.6262(7) 0.0804(5) 0.0281(12) Uani 1 1 d . . .
O3 O 0.5042(7) 0.2404(7) 0.0081(5) 0.0305(13) Uani 1 1 d . . .
O4 O 0.5369(7) 0.2655(7) 0.1868(4) 0.0249(12) Uani 1 1 d . . .
N1 N 0.4463(9) 0.4640(9) -0.2692(6) 0.0287(17) Uani 1 1 d . . .
N2 N 0.3388(8) 0.4268(9) -0.4446(5) 0.0249(14) Uani 1 1 d . . .
F1 F -0.1201(7) 0.7078(8) -0.0938(5) 0.0534(15) Uani 1 1 d . . .
F2 F -0.0944(8) 0.9162(8) -0.0687(7) 0.075(2) Uani 1 1 d . . .
F3 F -0.0837(7) 0.6927(9) 0.0869(5) 0.0672(18) Uani 1 1 d . . .
F4 F 0.4840(8) -0.0135(7) 0.2999(5) 0.0580(16) Uani 1 1 d . . .
F5 F 0.4823(9) -0.0561(8) 0.1387(6) 0.071(2) Uani 1 1 d . . .
F6 F 0.7243(8) -0.1152(8) 0.2339(6) 0.0697(19) Uani 1 1 d . . .
C1 C 0.1645(10) 0.6449(10) -0.0126(7) 0.0268(18) Uani 1 1 d . . .
C2 C -0.0360(11) 0.7402(13) -0.0209(8) 0.037(2) Uani 1 1 d . . .
C3 C 0.5273(10) 0.1868(11) 0.1224(7) 0.0272(17) Uani 1 1 d . . .
C4 C 0.5526(11) -0.0005(11) 0.1964(7) 0.0318(19) Uani 1 1 d . . .
C5 C 0.3865(10) 0.4534(10) -0.3504(7) 0.0222(16) Uani 1 1 d . . .
C6 C 0.1735(9) 0.4656(10) -0.4700(6) 0.0195(15) Uani 1 1 d . . .
C7 C 0.1297(10) 0.4181(10) -0.5650(6) 0.0224(17) Uani 1 1 d . . .
C8 C 0.0360(10) 0.5491(10) -0.4080(6) 0.0240(17) Uani 1 1 d . . .
H8 H 0.0642 0.5803 -0.3483 0.050 Uiso 1 1 calc . . .
C9 C 0.2743(11) 0.3265(12) -0.6243(8) 0.035(2) Uani 1 1 d . . .
H91 H 0.3831 0.3145 -0.5920 0.050 Uiso 1 1 calc . . .
H92 H 0.2461 0.3963 -0.7123 0.050 Uiso 1 1 calc . . .
H93 H 0.2866 0.2099 -0.6067 0.050 Uiso 1 1 calc . . .
C10 C 0.9551(17) 0.0111(16) 0.3856(10) 0.068(4) Uani 1 1 d . . .
H10 H 0.9264 0.0181 0.3079 0.050 Uiso 1 1 calc . . .
C11 C 0.8270(14) 0.0700(15) 0.4489(11) 0.061(3) Uani 1 1 d . . .
H11 H 0.7094 0.1173 0.4151 0.050 Uiso 1 1 calc . . .
C12 C 0.8694(14) 0.0604(15) 0.5627(10) 0.057(3) Uani 1 1 d . . .
H12 H 0.7804 0.1018 0.6059 0.050 Uiso 1 1 calc . . .
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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
O4 Rh1 O3 175.6(2) 2_665 . ?
O4 Rh1 O1 89.4(2) 2_665 . ?
O3 Rh1 O1 90.4(2) . . ?
O4 Rh1 O2 90.3(2) 2_665 2_665 ?
O3 Rh1 O2 89.6(2) . 2_665 ?
O1 Rh1 O2 175.66(19) . 2_665 ?
O4 Rh1 N1 92.1(2) 2_665 . ?
O3 Rh1 N1 92.3(2) . . ?
O1 Rh1 N1 91.2(2) . . ?
O2 Rh1 N1 93.1(2) 2_665 . ?
O4 Rh1 Rh1 88.06(14) 2_665 2_665 ?
O3 Rh1 Rh1 87.50(15) . 2_665 ?
O1 Rh1 Rh1 87.87(14) . 2_665 ?
O2 Rh1 Rh1 87.79(14) 2_665 2_665 ?
N1 Rh1 Rh1 179.05(19) . 2_665 ?
C1 O1 Rh1 117.1(5) . . ?
C1 O2 Rh1 116.9(5) . 2_665 ?
C3 O3 Rh1 118.1(5) . . ?
C3 O4 Rh1 117.4(5) . 2_665 ?
C5 N1 Rh1 161.9(6) . . ?
C6 N2 C5 118.3(6) . . ?
O1 C1 O2 130.3(7) . . ?
O1 C1 C2 116.0(7) . . ?
O2 C1 C2 113.7(7) . . ?
F3 C2 F1 106.9(7) . . ?
F3 C2 F2 108.2(8) . . ?
F1 C2 F2 107.1(7) . . ?
F3 C2 C1 112.6(7) . . ?
F1 C2 C1 112.3(7) . . ?
F2 C2 C1 109.6(7) . . ?
O3 C3 O4 129.0(7) . . ?
O3 C3 C4 116.5(7) . . ?
O4 C3 C4 114.5(6) . . ?
F5 C4 F6 108.8(7) . . ?
F5 C4 F4 106.2(7) . . ?
F6 C4 F4 105.6(7) . . ?
F5 C4 C3 114.6(7) . . ?
F6 C4 C3 109.8(7) . . ?
F4 C4 C3 111.5(7) . . ?
N1 C5 N2 172.6(9) . . ?
N2 C6 C8 123.7(6) . . ?
N2 C6 C7 116.8(6) . . ?
C8 C6 C7 119.5(6) . . ?
C8 C7 C6 119.0(7) 2_564 . ?
C8 C7 C9 122.3(7) 2_564 . ?
C6 C7 C9 118.6(6) . . ?
C7 C8 C6 121.5(6) 2_564 . ?
C11 C10 C12 119.4(11) . 2_756 ?
C10 C11 C12 120.2(9) . . ?
C11 C12 C10 120.3(11) . 2_756 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 O4 2.031(5) 2_665 ?
Rh1 O3 2.036(6) . ?
Rh1 O1 2.039(5) . ?
Rh1 O2 2.041(5) 2_665 ?
Rh1 N1 2.189(7) . ?
Rh1 Rh1 2.4125(14) 2_665 ?
O1 C1 1.241(9) . ?
O2 C1 1.247(9) . ?
O2 Rh1 2.041(5) 2_665 ?
O3 C3 1.240(9) . ?
O4 C3 1.258(9) . ?
O4 Rh1 2.031(5) 2_665 ?
N1 C5 1.157(9) . ?
N2 C6 1.310(9) . ?
N2 C5 1.337(9) . ?
F1 C2 1.328(9) . ?
F2 C2 1.329(10) . ?
F3 C2 1.305(10) . ?
F4 C4 1.338(9) . ?
F5 C4 1.282(9) . ?
F6 C4 1.333(10) . ?
C1 C2 1.531(11) . ?
C3 C4 1.509(11) . ?
C6 C8 1.453(10) . ?
C6 C7 1.462(9) . ?
C7 C8 1.334(10) 2_564 ?
C7 C9 1.494(11) . ?
C8 C7 1.334(10) 2_564 ?
C10 C11 1.347(16) . ?
C10 C12 1.391(14) 2_756 ?
C11 C12 1.366(16) . ?
C12 C10 1.391(14) 2_756 ?
