data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
loop_
_publ_author_name
S.Takamizawa
R.Miyake
_publ_contact_author_name        'Satoshi Takamizawa'
_publ_contact_author_email       STAKA@YOKOHAMA-CU.AC.JP

data_40414s1
_database_code_depnum_ccdc_archive 'CCDC 757356'
#TrackingRef 'staka-acetonitrile-cif.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H30 N4 O8 Rh2'
_chemical_formula_weight         852.46

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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.540(3)
_cell_length_b                   10.457(4)
_cell_length_c                   10.605(4)
_cell_angle_alpha                73.863(7)
_cell_angle_beta                 63.928(7)
_cell_angle_gamma                64.003(6)
_cell_volume                     849.4(5)
_cell_formula_units_Z            1
_cell_measurement_temperature    90
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8204
_exptl_absorpt_correction_T_max  0.8692
_exptl_absorpt_process_details   
;
SADABS; sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      90
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 8.366
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5517
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0867
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.15
_diffrn_reflns_theta_max         26.73
_reflns_number_total             3567
_reflns_number_gt                2730
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1050P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3567
_refine_ls_number_parameters     256
_refine_ls_number_restraints     333
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1965
_refine_ls_wR_factor_gt          0.1775
_refine_ls_goodness_of_fit_ref   1.185
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
C1 C 0.8227(8) 0.2534(8) 1.0891(8) 0.0168(14) Uani 1 1 d U . .
C2 C 0.7266(9) 0.4028(8) 1.1214(8) 0.0191(14) Uani 1 1 d U . .
C3 C 0.8051(9) 0.4862(8) 1.1255(8) 0.0222(15) Uani 1 1 d U . .
H3 H 0.9212 0.4453 1.1107 0.027 Uiso 1 1 calc R . .
C4 C 0.7153(10) 0.6277(9) 1.1510(9) 0.0261(16) Uani 1 1 d U . .
H4 H 0.7692 0.6844 1.1532 0.031 Uiso 1 1 calc R . .
C5 C 0.5446(10) 0.6869(9) 1.1735(9) 0.0280(17) Uani 1 1 d U . .
H5 H 0.4813 0.7833 1.1941 0.034 Uiso 1 1 calc R . .
C6 C 0.4680(10) 0.6061(9) 1.1659(9) 0.0271(17) Uani 1 1 d U . .
H6 H 0.3528 0.6483 1.1780 0.033 Uiso 1 1 calc R . .
C7 C 0.5563(9) 0.4642(8) 1.1410(8) 0.0219(15) Uani 1 1 d U . .
H7 H 0.5019 0.4088 1.1371 0.026 Uiso 1 1 calc R . .
C8 C 1.0426(9) 0.1321(8) 0.7457(8) 0.0195(14) Uani 1 1 d U . .
C9 C 1.0628(9) 0.2138(8) 0.6034(8) 0.0215(15) Uani 1 1 d U . .
C10 C 1.1619(10) 0.2967(9) 0.5475(9) 0.0280(17) Uani 1 1 d U . .
H10 H 1.2154 0.3030 0.6016 0.034 Uiso 1 1 calc R . .
C11 C 1.1835(11) 0.3703(10) 0.4137(10) 0.0350(19) Uani 1 1 d U . .
H11 H 1.2511 0.4269 0.3762 0.042 Uiso 1 1 calc R . .
C12 C 1.1045(10) 0.3600(10) 0.3349(9) 0.0315(18) Uani 1 1 d U . .
H12 H 1.1201 0.4086 0.2424 0.038 Uiso 1 1 calc R . .
C13 C 1.0043(10) 0.2803(10) 0.3903(9) 0.0303(18) Uani 1 1 d U . .
H13 H 0.9497 0.2751 0.3366 0.036 Uiso 1 1 calc R . .
C14 C 0.9826(10) 0.2070(9) 0.5249(9) 0.0279(17) Uani 1 1 d U . .
H14 H 0.9128 0.1524 0.5630 0.033 Uiso 1 1 calc R . .
C15 C 1.5047(8) -0.0589(7) 0.9016(8) 0.0174(14) Uani 1 1 d DU . .
H15 H 1.5130 -0.1014 0.8290 0.021 Uiso 1 1 calc R . .
C16 C 1.3504(9) 0.0689(8) 1.0903(8) 0.0182(15) Uani 1 1 d DU . .
H16 H 1.2452 0.1201 1.1561 0.022 Uiso 1 1 calc R . .
C1SA C 0.400(3) 0.878(2) 0.518(2) 0.039(5) Uani 0.436(13) 1 d PDU . .
C2SA C 0.476(4) 0.982(3) 0.488(3) 0.053(7) Uani 0.436(13) 1 d PDU . .
H1SA H 0.4924 0.9840 0.5723 0.080 Uiso 0.436(13) 1 calc PR . .
H2SA H 0.4031 1.0766 0.4618 0.080 Uiso 0.436(13) 1 calc PR . .
H3SA H 0.5851 0.9540 0.4101 0.080 Uiso 0.436(13) 1 calc PR . .
C1SB C 0.414(2) 0.697(2) 0.508(2) 0.051(4) Uani 0.564(13) 1 d PDU . .
C2SB C 0.482(3) 0.543(2) 0.502(3) 0.063(6) Uani 0.564(13) 1 d PDU . .
H1SB H 0.4321 0.4966 0.5953 0.094 Uiso 0.564(13) 1 calc PR . .
H2SB H 0.6039 0.5072 0.4757 0.094 Uiso 0.564(13) 1 calc PR . .
H3SB H 0.4557 0.5231 0.4323 0.094 Uiso 0.564(13) 1 calc PR . .
N1 N 1.3536(7) 0.0088(6) 0.9926(6) 0.0157(12) Uani 1 1 d DU . .
N1SA N 0.336(3) 0.797(3) 0.554(3) 0.051(5) Uani 0.436(13) 1 d PDU . .
N1SB N 0.359(3) 0.818(3) 0.507(2) 0.058(5) Uani 0.564(13) 1 d PDU . .
O1 O 0.9781(6) 0.2026(5) 1.0698(5) 0.0178(11) Uani 1 1 d U . .
O2 O 0.7465(6) 0.1851(5) 1.0790(6) 0.0188(11) Uani 1 1 d U . .
O3 O 1.1499(6) 0.1103(6) 0.7968(5) 0.0200(11) Uani 1 1 d U . .
O4 O 0.9191(6) 0.0922(6) 0.8055(6) 0.0199(11) Uani 1 1 d U . .
Rh1 Rh 1.12329(6) 0.00828(6) 0.99484(6) 0.0140(2) Uani 1 1 d U . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.016(2) 0.018(3) 0.016(3) -0.002(2) -0.006(2) -0.006(2)
C2 0.018(3) 0.019(3) 0.018(3) -0.001(2) -0.007(2) -0.004(2)
C3 0.021(3) 0.020(3) 0.023(3) 0.001(2) -0.007(2) -0.008(2)
C4 0.029(3) 0.019(3) 0.026(3) 0.002(2) -0.007(2) -0.010(2)
C5 0.030(3) 0.021(3) 0.026(3) 0.001(3) -0.008(3) -0.007(2)
C6 0.023(3) 0.026(3) 0.024(3) -0.001(3) -0.008(2) -0.002(2)
C7 0.021(3) 0.022(3) 0.021(3) -0.003(2) -0.006(2) -0.006(2)
C8 0.018(3) 0.018(3) 0.019(3) -0.003(2) -0.007(2) -0.003(2)
C9 0.021(3) 0.021(3) 0.021(3) -0.003(2) -0.006(2) -0.007(2)
C10 0.028(3) 0.025(3) 0.028(3) -0.001(3) -0.008(3) -0.010(2)
C11 0.034(3) 0.033(3) 0.031(3) 0.003(3) -0.007(3) -0.016(3)
C12 0.030(3) 0.033(3) 0.026(3) 0.000(3) -0.009(3) -0.010(3)
C13 0.031(3) 0.032(3) 0.027(3) -0.001(3) -0.013(3) -0.010(3)
C14 0.026(3) 0.031(3) 0.025(3) -0.003(3) -0.010(2) -0.009(2)
C15 0.019(3) 0.016(3) 0.021(3) -0.004(2) -0.006(2) -0.010(2)
C16 0.014(3) 0.018(3) 0.021(3) -0.005(2) -0.005(2) -0.004(2)
C1SA 0.039(6) 0.039(6) 0.038(6) -0.007(4) -0.015(4) -0.013(4)
C2SA 0.050(7) 0.049(7) 0.054(8) -0.007(4) -0.015(5) -0.017(5)
C1SB 0.050(5) 0.055(6) 0.052(6) -0.004(4) -0.022(4) -0.019(4)
C2SB 0.063(7) 0.062(7) 0.060(7) -0.006(5) -0.021(4) -0.023(5)
N1 0.013(2) 0.013(2) 0.019(3) -0.001(2) -0.006(2) -0.0038(19)
N1SA 0.053(6) 0.050(6) 0.050(6) -0.005(4) -0.018(4) -0.020(4)
N1SB 0.058(5) 0.056(6) 0.057(6) -0.007(4) -0.018(4) -0.021(4)
O1 0.013(2) 0.021(2) 0.022(2) -0.0030(19) -0.0072(18) -0.0060(17)
O2 0.014(2) 0.020(2) 0.024(2) -0.0049(19) -0.0075(19) -0.0059(18)
O3 0.019(2) 0.022(2) 0.020(2) 0.0017(19) -0.0078(19) -0.0102(18)
O4 0.017(2) 0.024(2) 0.020(2) 0.0001(19) -0.0074(19) -0.0090(18)
Rh1 0.0096(3) 0.0145(3) 0.0181(3) -0.0008(2) -0.0055(2) -0.0045(2)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
C1 O2 1.270(9) . ?
C1 O1 1.275(8) . ?
C1 C2 1.471(10) . ?
C2 C3 1.395(11) . ?
C2 C7 1.399(10) . ?
C3 C4 1.380(11) . ?
C4 C5 1.396(11) . ?
C5 C6 1.373(12) . ?
C6 C7 1.381(11) . ?
C8 O4 1.261(9) . ?
C8 O3 1.267(9) . ?
C8 C9 1.489(11) . ?
C9 C14 1.387(12) . ?
C9 C10 1.392(11) . ?
C10 C11 1.386(12) . ?
C11 C12 1.397(13) . ?
C12 C13 1.373(12) . ?
C13 C14 1.393(12) . ?
C15 N1 1.332(7) . ?
C15 C16 1.378(10) 2_857 ?
C16 N1 1.337(7) . ?
C16 C15 1.378(10) 2_857 ?
C1SA N1SA 1.14(3) . ?
C1SA C2SA 1.45(2) . ?
C1SB N1SB 1.14(3) . ?
C1SB C2SB 1.45(2) . ?
N1 Rh1 2.189(6) . ?
O1 Rh1 2.036(5) . ?
O2 Rh1 2.018(5) 2_757 ?
O3 Rh1 2.034(5) . ?
O4 Rh1 2.033(5) 2_757 ?
Rh1 O2 2.018(5) 2_757 ?
Rh1 O4 2.033(5) 2_757 ?
Rh1 Rh1 2.3866(13) 2_757 ?

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
O2 C1 O1 124.6(7) . . ?
O2 C1 C2 118.0(6) . . ?
O1 C1 C2 117.4(6) . . ?
C3 C2 C7 119.6(7) . . ?
C3 C2 C1 120.8(6) . . ?
C7 C2 C1 119.6(7) . . ?
C4 C3 C2 120.4(7) . . ?
C3 C4 C5 119.5(8) . . ?
C6 C5 C4 120.2(8) . . ?
C5 C6 C7 120.9(7) . . ?
C6 C7 C2 119.4(8) . . ?
O4 C8 O3 125.8(7) . . ?
O4 C8 C9 117.1(7) . . ?
O3 C8 C9 117.1(6) . . ?
C14 C9 C10 119.3(8) . . ?
C14 C9 C8 119.8(7) . . ?
C10 C9 C8 120.9(7) . . ?
C11 C10 C9 120.8(8) . . ?
C10 C11 C12 119.1(8) . . ?
C13 C12 C11 120.4(9) . . ?
C12 C13 C14 120.3(9) . . ?
C9 C14 C13 120.1(8) . . ?
N1 C15 C16 121.8(6) . 2_857 ?
N1 C16 C15 122.0(6) . 2_857 ?
N1SA C1SA C2SA 174(3) . . ?
N1SB C1SB C2SB 177(3) . . ?
C15 N1 C16 116.1(6) . . ?
C15 N1 Rh1 122.5(5) . . ?
C16 N1 Rh1 121.2(4) . . ?
C1 O1 Rh1 118.6(5) . . ?
C1 O2 Rh1 120.2(4) . 2_757 ?
C8 O3 Rh1 119.2(5) . . ?
C8 O4 Rh1 118.8(5) . 2_757 ?
O2 Rh1 O4 88.8(2) 2_757 2_757 ?
O2 Rh1 O3 91.8(2) 2_757 . ?
O4 Rh1 O3 176.09(19) 2_757 . ?
O2 Rh1 O1 176.23(19) 2_757 . ?
O4 Rh1 O1 91.1(2) 2_757 . ?
O3 Rh1 O1 88.0(2) . . ?
O2 Rh1 N1 89.57(19) 2_757 . ?
O4 Rh1 N1 88.7(2) 2_757 . ?
O3 Rh1 N1 95.2(2) . . ?
O1 Rh1 N1 94.20(19) . . ?
O2 Rh1 Rh1 87.86(14) 2_757 2_757 ?
O4 Rh1 Rh1 88.38(14) 2_757 2_757 ?
O3 Rh1 Rh1 87.78(14) . 2_757 ?
O1 Rh1 Rh1 88.37(14) . 2_757 ?
N1 Rh1 Rh1 176.15(15) . 2_757 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 C1 C2 C3 -176.1(7) . . . . ?
O1 C1 C2 C3 2.3(11) . . . . ?
O2 C1 C2 C7 0.5(11) . . . . ?
O1 C1 C2 C7 178.9(7) . . . . ?
C7 C2 C3 C4 1.1(12) . . . . ?
C1 C2 C3 C4 177.7(7) . . . . ?
C2 C3 C4 C5 0.4(12) . . . . ?
C3 C4 C5 C6 -2.0(12) . . . . ?
C4 C5 C6 C7 2.3(13) . . . . ?
C5 C6 C7 C2 -0.8(12) . . . . ?
C3 C2 C7 C6 -0.9(11) . . . . ?
C1 C2 C7 C6 -177.5(7) . . . . ?
O4 C8 C9 C14 -19.1(11) . . . . ?
O3 C8 C9 C14 161.7(7) . . . . ?
O4 C8 C9 C10 161.1(7) . . . . ?
O3 C8 C9 C10 -18.0(11) . . . . ?
C14 C9 C10 C11 -1.1(12) . . . . ?
C8 C9 C10 C11 178.6(8) . . . . ?
C9 C10 C11 C12 -0.1(13) . . . . ?
C10 C11 C12 C13 1.2(14) . . . . ?
C11 C12 C13 C14 -1.0(14) . . . . ?
C10 C9 C14 C13 1.3(12) . . . . ?
C8 C9 C14 C13 -178.4(7) . . . . ?
C12 C13 C14 C9 -0.3(13) . . . . ?
C16 C15 N1 C16 1.3(11) 2_857 . . . ?
C16 C15 N1 Rh1 -173.8(5) 2_857 . . . ?
C15 C16 N1 C15 -1.4(11) 2_857 . . . ?
C15 C16 N1 Rh1 173.9(5) 2_857 . . . ?
O2 C1 O1 Rh1 7.8(10) . . . . ?
C2 C1 O1 Rh1 -170.5(5) . . . . ?
O1 C1 O2 Rh1 -7.9(10) . . . 2_757 ?
C2 C1 O2 Rh1 170.3(5) . . . 2_757 ?
O4 C8 O3 Rh1 -2.2(10) . . . . ?
C9 C8 O3 Rh1 176.9(5) . . . . ?
O3 C8 O4 Rh1 3.1(10) . . . 2_757 ?
C9 C8 O4 Rh1 -176.0(5) . . . 2_757 ?
C8 O3 Rh1 O2 88.1(5) . . . 2_757 ?
C8 O3 Rh1 O4 -10(4) . . . 2_757 ?
C8 O3 Rh1 O1 -88.1(6) . . . . ?
C8 O3 Rh1 N1 177.8(5) . . . . ?
C8 O3 Rh1 Rh1 0.3(5) . . . 2_757 ?
C1 O1 Rh1 O2 -3(3) . . . 2_757 ?
C1 O1 Rh1 O4 -91.9(5) . . . 2_757 ?
C1 O1 Rh1 O3 84.3(5) . . . . ?
C1 O1 Rh1 N1 179.3(5) . . . . ?
C1 O1 Rh1 Rh1 -3.6(5) . . . 2_757 ?
C15 N1 Rh1 O2 29.3(6) . . . 2_757 ?
C16 N1 Rh1 O2 -145.7(6) . . . 2_757 ?
C15 N1 Rh1 O4 118.1(6) . . . 2_757 ?
C16 N1 Rh1 O4 -56.8(6) . . . 2_757 ?
C15 N1 Rh1 O3 -62.5(6) . . . . ?
C16 N1 Rh1 O3 122.6(6) . . . . ?
C15 N1 Rh1 O1 -150.9(6) . . . . ?
C16 N1 Rh1 O1 34.2(6) . . . . ?
C15 N1 Rh1 Rh1 77(2) . . . 2_757 ?
C16 N1 Rh1 Rh1 -98(2) . . . 2_757 ?

_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full        26.73
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max         1.921
_refine_diff_density_min         -2.497
_refine_diff_density_rms         0.356