 
data_40
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C32 H36 N4 O14 Rh2' 
_chemical_formula_sum 
 'C32 H36 N4 O14 Rh2' 
_chemical_formula_weight          906.47 
  
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' 
  
_space_group_crystal_system       triclinic 
_space_group_IT_number            2 
_space_group_name_H-M_alt         'P -1' 
_space_group_name_Hall            '-P 1' 
  
_shelx_space_group_comment 
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
; 
  
loop_ 
 _space_group_symop_operation_xyz 
 'x, y, z' 
 '-x, -y, -z' 
  
_cell_length_a                    9.4423(6) 
_cell_length_b                    9.8753(5) 
_cell_length_c                    11.5911(6) 
_cell_angle_alpha                 108.310(5) 
_cell_angle_beta                  95.302(5) 
_cell_angle_gamma                 114.600(5) 
_cell_volume                      901.23(9) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     4571 
_cell_measurement_theta_min       4.1330 
_cell_measurement_theta_max       73.3600 
  
_exptl_crystal_description        blocks 
_exptl_crystal_colour             'Purple dichroic' 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.670 
_exptl_crystal_F_000              458 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.191 
_exptl_crystal_size_mid           0.095 
_exptl_crystal_size_min           0.053 
_exptl_absorpt_coefficient_mu     8.039 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.444 
_exptl_absorpt_correction_T_max   0.742 
_exptl_absorpt_process_details     
; 
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
; 
_exptl_absorpt_special_details    ? 
_diffrn_ambient_temperature       173(2) 
_diffrn_radiation_wavelength      1.54184 
_diffrn_radiation_type            CuK\a 
_diffrn_source                    'Enhance Ultra (Cu) X-ray Source' 
_diffrn_measurement_device_type   'Agilent Xcalibur PX Ultra A' 
_diffrn_measurement_method        'omega scans' 
_diffrn_detector_area_resol_mean  10.4115 
_diffrn_reflns_number             9928 
_diffrn_reflns_av_unetI/netI      0.0421 
_diffrn_reflns_av_R_equivalents   0.0367 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -14 
_diffrn_reflns_limit_l_max        13 
_diffrn_reflns_theta_min          4.159 
_diffrn_reflns_theta_max          73.670 
_diffrn_reflns_theta_full         67.684 
_diffrn_measured_fraction_theta_max   0.972 
_diffrn_measured_fraction_theta_full  0.994 
_diffrn_reflns_Laue_measured_fraction_max    0.972 
_diffrn_reflns_Laue_measured_fraction_full   0.994 
_diffrn_reflns_point_group_measured_fraction_max   0.972 
_diffrn_reflns_point_group_measured_fraction_full  0.994 
_reflns_number_total              3546 
_reflns_number_gt                 2984 
_reflns_threshold_expression      'I > 2σ(I)' 
_reflns_Friedel_coverage          0.000 
_reflns_Friedel_fraction_max      . 
_reflns_Friedel_fraction_full     . 
  
_reflns_special_details 
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
; 
  
_computing_data_collection        'CrysAlisPro, Rigaku OD' 
_computing_cell_refinement        'CrysAlisPro, Rigaku OD' 
_computing_data_reduction         'CrysAlisPro, Rigaku OD' 
_computing_structure_solution     'SHELXS-2014 (Sheldrick, 2017)' 
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' 
_computing_molecular_graphics     'Bruker SHELXTL' 
_computing_publication_material   'CIFTAB-2014 (Sheldrick, 2017)' 
_refine_special_details           ? 
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
'w=1/[σ²(Fo²)+(0.0097P)²+1.1205P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      ? 
_atom_sites_solution_secondary    ? 
_atom_sites_solution_hydrogens    mixed 
_refine_ls_hydrogen_treatment     mixed 
_refine_ls_extinction_method      'SHELXL-2018/3 (Sheldrick 2018)' 
_refine_ls_extinction_coef        0.00032(5) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          3546 
_refine_ls_number_parameters      243 
_refine_ls_number_restraints      1 
_refine_ls_R_factor_all           0.0418 
_refine_ls_R_factor_gt            0.0297 
_refine_ls_wR_factor_ref          0.0619 
_refine_ls_wR_factor_gt           0.0559 
_refine_ls_goodness_of_fit_ref    1.053 
_refine_ls_restrained_S_all       1.053 
_refine_ls_shift/su_max           0.001 
_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_site_symmetry_order 
 _atom_site_calc_flag 
 _atom_site_refinement_flags_posn 
 _atom_site_refinement_flags_adp 
 _atom_site_refinement_flags_occupancy 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Rh1 Rh 0.05963(3) 0.13389(3) 0.58032(2) 0.02559(8) Uani 1 1 d . . . . . 
N1 N 0.1801(3) 0.3879(3) 0.7331(2) 0.0229(6) Uani 1 1 d . . . . . 
N2 N 0.1294(3) 0.5028(3) 0.7628(3) 0.0294(7) Uani 1 1 d . . . . . 
C3 C 0.2512(4) 0.6470(4) 0.8438(3) 0.0285(7) Uani 1 1 d . . . . . 
O3 O 0.2253(3) 0.7741(3) 0.8856(2) 0.0428(7) Uani 1 1 d D . . . . 
H3 H 0.3184(6) 0.8597(10) 0.9369(10) 0.056(13) Uiso 1 1 d D . . . . 
C4 C 0.3865(4) 0.6270(4) 0.8676(3) 0.0292(7) Uani 1 1 d . . . . . 
C5 C 0.3331(4) 0.4617(4) 0.7955(3) 0.0289(7) Uani 1 1 d . . . . . 
H5A H 0.398992 0.410315 0.792244 0.035 Uiso 1 1 calc R U . . . 
C6 C -0.0362(4) 0.4630(4) 0.7196(3) 0.0298(8) Uani 1 1 d . . . . . 
C7 C -0.1526(4) 0.3606(4) 0.7592(4) 0.0361(8) Uani 1 1 d . . . . . 
H7A H -0.124296 0.316747 0.814105 0.043 Uiso 1 1 calc R U . . . 
C8 C -0.3122(4) 0.3228(5) 0.7169(4) 0.0447(10) Uani 1 1 d . . . . . 
H8A H -0.394169 0.252823 0.743330 0.054 Uiso 1 1 calc R U . . . 
C9 C -0.3520(5) 0.3864(5) 0.6370(4) 0.0440(10) Uani 1 1 d . . . . . 
H9A H -0.461529 0.359362 0.608025 0.053 Uiso 1 1 calc R U . . . 
C10 C -0.2339(5) 0.4894(5) 0.5984(4) 0.0421(9) Uani 1 1 d . . . . . 
H10A H -0.262334 0.532458 0.542881 0.051 Uiso 1 1 calc R U . . . 
C11 C -0.0738(4) 0.5299(4) 0.6410(3) 0.0353(8) Uani 1 1 d . . . . . 
H11A H 0.008495 0.602310 0.616457 0.042 Uiso 1 1 calc R U . . . 
C12 C 0.5400(4) 0.7541(4) 0.9502(3) 0.0295(8) Uani 1 1 d . . . . . 
O12 O 0.5649(3) 0.8925(3) 1.0054(2) 0.0426(7) Uani 1 1 d . . . . . 
O13 O 0.6503(3) 0.7047(3) 0.9585(2) 0.0327(6) Uani 1 1 d . . . . . 
C14 C 0.8110(4) 0.8241(4) 1.0383(3) 0.0351(8) Uani 1 1 d . . . . . 
H14A H 0.811340 0.850898 1.128104 0.042 Uiso 1 1 calc R U . . . 
H14B H 0.847555 0.924515 1.022125 0.042 Uiso 1 1 calc R U . . . 
C15 C 0.9184(5) 0.7506(5) 1.0064(4) 0.0465(10) Uani 1 1 d . . . . . 
H15A H 0.923653 0.732836 0.919161 0.070 Uiso 1 1 calc R U . . . 
H15B H 0.875722 0.646965 1.016144 0.070 Uiso 1 1 calc R U . . . 
H15C H 1.026806 0.823498 1.062839 0.070 Uiso 1 1 calc R U . . . 
O20 O 0.2120(3) 0.2097(3) 0.4743(2) 0.0301(5) Uani 1 1 d . . . . . 
C21 C 0.1977(4) 0.1077(4) 0.3692(3) 0.0287(7) Uani 1 1 d . . . . . 
O22 O 0.0968(3) -0.0407(3) 0.3216(2) 0.0305(5) Uani 1 1 d . . . . . 
C23 C 0.3100(5) 0.1703(5) 0.2928(3) 0.0390(9) Uani 1 1 d . . . . . 
H23A H 0.319972 0.080895 0.233526 0.059 Uiso 1 1 calc R U . . . 
H23B H 0.416301 0.252724 0.348998 0.059 Uiso 1 1 calc R U . . . 
H23C H 0.266834 0.217991 0.246089 0.059 Uiso 1 1 calc R U . . . 
O30 O 0.2260(3) 0.0857(3) 0.6604(2) 0.0292(5) Uani 1 1 d . . . . . 
C31 C 0.2165(4) -0.0522(4) 0.6075(3) 0.0275(7) Uani 1 1 d . . . . . 
O32 O 0.1088(3) -0.1677(3) 0.5118(2) 0.0309(5) Uani 1 1 d . . . . . 
C33 C 0.3469(4) -0.0819(5) 0.6616(3) 0.0383(9) Uani 1 1 d . . . . . 
H33A H 0.303517 -0.197308 0.644435 0.057 Uiso 1 1 calc R U . . . 
H33B H 0.385480 -0.019480 0.752640 0.057 Uiso 1 1 calc R U . . . 
H33C H 0.436632 -0.048222 0.622736 0.057 Uiso 1 1 calc R U . . . 
  
  
_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 
Rh1 O32 2.033(2) 2_556 ? 
Rh1 O20 2.037(2) . ? 
Rh1 O22 2.039(2) 2_556 ? 
Rh1 O30 2.045(2) . ? 
Rh1 N1 2.276(2) . ? 
Rh1 Rh1 2.4015(5) 2_556 ? 
N1 C5 1.319(4) . ? 
N1 N2 1.369(3) . ? 
N2 C3 1.352(4) . ? 
N2 C6 1.438(4) . ? 
C3 O3 1.328(4) . ? 
C3 C4 1.389(5) . ? 
C4 C5 1.413(4) . ? 
C4 C12 1.437(4) . ? 
C6 C7 1.378(5) . ? 
C6 C11 1.381(5) . ? 
C7 C8 1.390(5) . ? 
C8 C9 1.375(6) . ? 
C9 C10 1.382(6) . ? 
C10 C11 1.387(5) . ? 
C12 O12 1.220(4) . ? 
C12 O13 1.329(4) . ? 
O13 C14 1.454(4) . ? 
C14 C15 1.486(5) . ? 
O20 C21 1.266(4) . ? 
C21 O22 1.262(4) . ? 
C21 C23 1.504(5) . ? 
O30 C31 1.266(4) . ? 
C31 O32 1.263(4) . ? 
C31 C33 1.506(5) . ? 
  
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 
O32 Rh1 O20 91.21(10) 2_556 . ? 
O32 Rh1 O22 89.79(10) 2_556 2_556 ? 
O20 Rh1 O22 175.70(9) . 2_556 ? 
O32 Rh1 O30 175.58(9) 2_556 . ? 
O20 Rh1 O30 87.09(9) . . ? 
O22 Rh1 O30 91.61(10) 2_556 . ? 
O32 Rh1 N1 94.13(9) 2_556 . ? 
O20 Rh1 N1 90.90(9) . . ? 
O22 Rh1 N1 93.20(9) 2_556 . ? 
O30 Rh1 N1 89.98(9) . . ? 
O32 Rh1 Rh1 87.34(6) 2_556 2_556 ? 
O20 Rh1 Rh1 88.13(6) . 2_556 ? 
O22 Rh1 Rh1 87.74(6) 2_556 2_556 ? 
O30 Rh1 Rh1 88.52(6) . 2_556 ? 
N1 Rh1 Rh1 178.26(7) . 2_556 ? 
C5 N1 N2 106.2(2) . . ? 
C5 N1 Rh1 122.5(2) . . ? 
N2 N1 Rh1 130.26(19) . . ? 
C3 N2 N1 110.4(3) . . ? 
C3 N2 C6 127.5(3) . . ? 
N1 N2 C6 121.9(3) . . ? 
O3 C3 N2 119.6(3) . . ? 
O3 C3 C4 132.4(3) . . ? 
N2 C3 C4 107.9(3) . . ? 
C3 C4 C5 104.0(3) . . ? 
C3 C4 C12 124.1(3) . . ? 
C5 C4 C12 131.9(3) . . ? 
N1 C5 C4 111.5(3) . . ? 
C7 C6 C11 121.9(3) . . ? 
C7 C6 N2 119.0(3) . . ? 
C11 C6 N2 119.2(3) . . ? 
C6 C7 C8 118.6(4) . . ? 
C9 C8 C7 120.3(4) . . ? 
C8 C9 C10 120.5(4) . . ? 
C9 C10 C11 119.9(4) . . ? 
C6 C11 C10 118.8(4) . . ? 
O12 C12 O13 124.2(3) . . ? 
O12 C12 C4 122.9(3) . . ? 
O13 C12 C4 112.9(3) . . ? 
C12 O13 C14 117.6(3) . . ? 
O13 C14 C15 106.5(3) . . ? 
C21 O20 Rh1 118.7(2) . . ? 
O22 C21 O20 126.3(3) . . ? 
O22 C21 C23 116.9(3) . . ? 
O20 C21 C23 116.8(3) . . ? 
C21 O22 Rh1 119.1(2) . 2_556 ? 
C31 O30 Rh1 118.0(2) . . ? 
O32 C31 O30 126.2(3) . . ? 
O32 C31 C33 116.3(3) . . ? 
O30 C31 C33 117.5(3) . . ? 
C31 O32 Rh1 119.8(2) . 2_556 ? 
  
loop_ 
 _geom_hbond_atom_site_label_D 
 _geom_hbond_atom_site_label_H 
 _geom_hbond_atom_site_label_A 
 _geom_hbond_distance_DH 
 _geom_hbond_distance_HA 
 _geom_hbond_distance_DA 
 _geom_hbond_angle_DHA 
 _geom_hbond_site_symmetry_A 
 _geom_hbond_publ_flag 
O3 H3 O12  0.9000(2) 2.241(9) 2.934(3) 133.5(9) . yes 
O3 H3 O12  0.9000(2) 2.059(9) 2.803(3) 139.2(11) 2_677 yes 
  
_refine_diff_density_max    0.448 
_refine_diff_density_min   -0.545 
_refine_diff_density_rms    0.084 
  
  
  
#===END

