 
data_39
  
_audit_creation_method            'SHELXL-2018/3' 
_shelx_SHELXL_version_number      '2018/3' 
_chemical_name_systematic         ? 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety
 'C36 H44 N4 O16 Rh2' 
_chemical_formula_sum 
 'C36 H44 N4 O16 Rh2' 
_chemical_formula_weight          994.57 
  
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                    8.1670(4) 
_cell_length_b                    8.8751(4) 
_cell_length_c                    14.4104(6) 
_cell_angle_alpha                 81.575(4) 
_cell_angle_beta                  79.844(4) 
_cell_angle_gamma                 85.308(4) 
_cell_volume                      1015.36(8) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     5950 
_cell_measurement_theta_min       5.0160 
_cell_measurement_theta_max       72.7070 
  
_exptl_crystal_description        plates 
_exptl_crystal_colour             Purple 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.627 
_exptl_crystal_F_000              506 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.206 
_exptl_crystal_size_mid           0.142 
_exptl_crystal_size_min           0.017 
_exptl_absorpt_coefficient_mu     7.231 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.372 
_exptl_absorpt_correction_T_max   0.882 
_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             16749 
_diffrn_reflns_av_unetI/netI      0.0398 
_diffrn_reflns_av_R_equivalents   0.0488 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        -17 
_diffrn_reflns_limit_l_max        17 
_diffrn_reflns_theta_min          5.046 
_diffrn_reflns_theta_max          73.823 
_diffrn_reflns_theta_full         67.684 
_diffrn_measured_fraction_theta_max   0.982 
_diffrn_measured_fraction_theta_full  0.999 
_diffrn_reflns_Laue_measured_fraction_max    0.982 
_diffrn_reflns_Laue_measured_fraction_full   0.999 
_diffrn_reflns_point_group_measured_fraction_max   0.982 
_diffrn_reflns_point_group_measured_fraction_full  0.999 
_reflns_number_total              4035 
_reflns_number_gt                 3375 
_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)+(0.0207P)²+0.9184P] 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      none 
_refine_ls_extinction_coef        . 
_refine_ls_number_reflns          4035 
_refine_ls_number_parameters      278 
_refine_ls_number_restraints      22 
_refine_ls_R_factor_all           0.0464 
_refine_ls_R_factor_gt            0.0331 
_refine_ls_wR_factor_ref          0.0737 
_refine_ls_wR_factor_gt           0.0671 
_refine_ls_goodness_of_fit_ref    1.057 
_refine_ls_restrained_S_all       1.061 
_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 0.94045(3) 0.95970(3) 0.08107(2) 0.03738(9) Uani 1 1 d . . . . . 
N1 N 0.8220(4) 0.9052(3) 0.23661(18) 0.0387(7) Uani 1 1 d . . . . . 
N2 N 0.7908(4) 0.7723(3) 0.2947(2) 0.0433(7) Uani 1 1 d . . . . . 
C3 C 0.7443(5) 0.7996(5) 0.3841(3) 0.0511(10) Uani 1 1 d . . . . . 
O3 O 0.7067(4) 0.6833(3) 0.45437(16) 0.0677(9) Uani 1 1 d D . . . . 
H3 H 0.687(9) 0.7264(6) 0.5084(2) 0.17(3) Uiso 1 1 d D . . . . 
C4 C 0.7437(5) 0.9543(5) 0.3875(3) 0.0520(10) Uani 1 1 d . . . . . 
C5 C 0.7931(5) 1.0149(5) 0.2925(3) 0.0506(10) Uani 1 1 d . . . . . 
H5A H 0.804491 1.120392 0.270554 0.061 Uiso 1 1 calc R U . . . 
C6 C 0.7990(5) 0.6274(4) 0.2577(3) 0.0488(9) Uani 1 1 d . . . . . 
H6A H 0.857236 0.548761 0.298253 0.059 Uiso 1 1 calc R U . . . 
H6B H 0.865233 0.637639 0.192752 0.059 Uiso 1 1 calc R U . . . 
C7 C 0.6290(4) 0.5753(4) 0.2540(2) 0.0401(8) Uani 1 1 d . . . . . 
C8 C 0.5172(5) 0.6676(4) 0.2059(3) 0.0452(9) Uani 1 1 d . . . . . 
H8A H 0.546765 0.766422 0.175773 0.054 Uiso 1 1 calc R U . . . 
C9 C 0.3646(5) 0.6185(5) 0.2012(3) 0.0503(9) Uani 1 1 d . . . . . 
H9A H 0.287926 0.683712 0.169311 0.060 Uiso 1 1 calc R U . . . 
C10 C 0.3222(5) 0.4718(5) 0.2436(3) 0.0492(9) Uani 1 1 d . . . . . 
C11 C 0.4310(5) 0.3780(4) 0.2910(3) 0.0500(9) Uani 1 1 d . . . . . 
H11A H 0.402562 0.278223 0.319878 0.060 Uiso 1 1 calc R U . . . 
C12 C 0.5841(5) 0.4320(4) 0.2960(2) 0.0453(9) Uani 1 1 d . . . . . 
H12A H 0.659709 0.367991 0.329397 0.054 Uiso 1 1 calc R U . . . 
O13 O 0.1675(4) 0.4326(4) 0.2334(2) 0.0722(9) Uani 1 1 d . . . . . 
C14 C 0.1079(6) 0.2934(6) 0.2851(4) 0.0822(16) Uani 1 1 d . . . . . 
H14A H 0.185062 0.208368 0.266485 0.123 Uiso 1 1 calc R U . . . 
H14B H -0.002424 0.278941 0.270974 0.123 Uiso 1 1 calc R U . . . 
H14C H 0.099864 0.296844 0.353404 0.123 Uiso 1 1 calc R U . . . 
C15 C 0.7099(6) 1.0157(5) 0.4770(3) 0.0636(12) Uani 1 1 d . . . . . 
O15 O 0.6727(5) 0.9346(4) 0.5530(2) 0.0797(10) Uani 1 1 d . . . . . 
O16 O 0.7249(5) 1.1656(4) 0.4685(2) 0.0780(10) Uani 1 1 d D . . . . 
C17 C 0.6958(8) 1.2446(9) 0.5536(4) 0.0561(18) Uani 0.716(11) 1 d D U P A 1 
H17A H 0.615149 1.191098 0.604728 0.067 Uiso 0.716(11) 1 calc R U P A 1 
H17B H 0.651921 1.351004 0.538244 0.067 Uiso 0.716(11) 1 calc R U P A 1 
C18 C 0.8627(9) 1.2414(13) 0.5835(6) 0.091(3) Uani 0.716(11) 1 d D U P A 1 
H18A H 0.852200 1.292556 0.640238 0.137 Uiso 0.716(11) 1 calc R U P A 1 
H18B H 0.904267 1.135325 0.597906 0.137 Uiso 0.716(11) 1 calc R U P A 1 
H18C H 0.940819 1.294275 0.531820 0.137 Uiso 0.716(11) 1 calc R U P A 1 
C17' C 0.759(3) 1.1927(18) 0.5667(10) 0.057(4) Uiso 0.284(11) 1 d D U P A 2 
H17C H 0.655567 1.189765 0.614269 0.069 Uiso 0.284(11) 1 calc R U P A 2 
H17D H 0.842523 1.115668 0.589812 0.069 Uiso 0.284(11) 1 calc R U P A 2 
C18' C 0.824(3) 1.347(2) 0.5471(14) 0.080(6) Uiso 0.284(11) 1 d D U P A 2 
H18D H 0.850031 1.375193 0.605858 0.120 Uiso 0.284(11) 1 calc R U P A 2 
H18E H 0.925289 1.346777 0.499146 0.120 Uiso 0.284(11) 1 calc R U P A 2 
H18F H 0.739804 1.420290 0.523410 0.120 Uiso 0.284(11) 1 calc R U P A 2 
O20 O 0.7421(3) 0.8950(3) 0.03212(17) 0.0434(6) Uani 1 1 d . . . . . 
C21 C 0.7405(4) 0.9127(4) -0.0567(3) 0.0427(8) Uani 1 1 d . . . . . 
O22 O 0.8525(3) 0.9726(3) -0.12080(17) 0.0463(6) Uani 1 1 d . . . . . 
C23 C 0.5928(5) 0.8566(5) -0.0876(3) 0.0587(11) Uani 1 1 d . . . . . 
H23A H 0.570484 0.919622 -0.146312 0.088 Uiso 1 1 calc R U . . . 
H23B H 0.495228 0.863357 -0.037642 0.088 Uiso 1 1 calc R U . . . 
H23C H 0.616426 0.750248 -0.099118 0.088 Uiso 1 1 calc R U . . . 
O30 O 1.0555(3) 0.7493(3) 0.06395(16) 0.0421(6) Uani 1 1 d . . . . . 
C31 C 1.1408(4) 0.7271(4) -0.0155(2) 0.0406(8) Uani 1 1 d . . . . . 
O32 O 1.1658(3) 0.8260(3) -0.08824(16) 0.0430(6) Uani 1 1 d . . . . . 
C33 C 1.2210(5) 0.5691(4) -0.0241(3) 0.0527(10) Uani 1 1 d . . . . . 
H33A H 1.148683 0.509918 -0.050573 0.079 Uiso 1 1 calc R U . . . 
H33B H 1.237364 0.518140 0.038979 0.079 Uiso 1 1 calc R U . . . 
H33C H 1.329048 0.576898 -0.066177 0.079 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 O20 2.031(2) . ? 
Rh1 O32 2.034(2) 2_775 ? 
Rh1 O22 2.039(2) 2_775 ? 
Rh1 O30 2.049(2) . ? 
Rh1 N1 2.278(3) . ? 
Rh1 Rh1 2.3956(5) 2_775 ? 
N1 C5 1.332(4) . ? 
N1 N2 1.357(4) . ? 
N2 C3 1.329(5) . ? 
N2 C6 1.455(5) . ? 
C3 O3 1.349(4) . ? 
C3 C4 1.380(6) . ? 
C4 C5 1.397(5) . ? 
C4 C15 1.447(5) . ? 
C6 C7 1.511(5) . ? 
C7 C12 1.375(5) . ? 
C7 C8 1.386(5) . ? 
C8 C9 1.369(5) . ? 
C9 C10 1.397(5) . ? 
C10 C11 1.370(6) . ? 
C10 O13 1.375(4) . ? 
C11 C12 1.392(5) . ? 
O13 C14 1.421(5) . ? 
C15 O15 1.224(5) . ? 
C15 O16 1.332(5) . ? 
O16 C17 1.475(5) . ? 
O16 C17' 1.545(14) . ? 
C17 C18 1.497(9) . ? 
C17' C18' 1.477(16) . ? 
O20 C21 1.269(4) . ? 
C21 O22 1.269(4) . ? 
C21 C23 1.501(5) . ? 
O30 C31 1.263(4) . ? 
C31 O32 1.264(4) . ? 
C31 C33 1.510(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 
O20 Rh1 O32 91.35(10) . 2_775 ? 
O20 Rh1 O22 176.09(10) . 2_775 ? 
O32 Rh1 O22 89.07(10) 2_775 2_775 ? 
O20 Rh1 O30 88.69(10) . . ? 
O32 Rh1 O30 175.84(9) 2_775 . ? 
O22 Rh1 O30 90.61(10) 2_775 . ? 
O20 Rh1 N1 93.53(10) . . ? 
O32 Rh1 N1 86.38(10) 2_775 . ? 
O22 Rh1 N1 90.38(10) 2_775 . ? 
O30 Rh1 N1 97.77(10) . . ? 
O20 Rh1 Rh1 87.76(7) . 2_775 ? 
O32 Rh1 Rh1 88.70(7) 2_775 2_775 ? 
O22 Rh1 Rh1 88.36(7) 2_775 2_775 ? 
O30 Rh1 Rh1 87.14(6) . 2_775 ? 
N1 Rh1 Rh1 174.94(8) . 2_775 ? 
C5 N1 N2 106.1(3) . . ? 
C5 N1 Rh1 120.2(2) . . ? 
N2 N1 Rh1 132.9(2) . . ? 
C3 N2 N1 109.9(3) . . ? 
C3 N2 C6 128.1(3) . . ? 
N1 N2 C6 121.8(3) . . ? 
N2 C3 O3 120.2(4) . . ? 
N2 C3 C4 109.4(3) . . ? 
O3 C3 C4 130.4(3) . . ? 
C3 C4 C5 103.4(3) . . ? 
C3 C4 C15 121.4(4) . . ? 
C5 C4 C15 134.9(4) . . ? 
N1 C5 C4 111.1(3) . . ? 
N2 C6 C7 112.7(3) . . ? 
C12 C7 C8 118.4(3) . . ? 
C12 C7 C6 120.3(3) . . ? 
C8 C7 C6 121.2(3) . . ? 
C9 C8 C7 121.0(3) . . ? 
C8 C9 C10 119.6(4) . . ? 
C11 C10 O13 124.4(4) . . ? 
C11 C10 C9 120.5(4) . . ? 
O13 C10 C9 115.1(4) . . ? 
C10 C11 C12 118.6(4) . . ? 
C7 C12 C11 121.9(4) . . ? 
C10 O13 C14 117.9(4) . . ? 
O15 C15 O16 124.1(4) . . ? 
O15 C15 C4 121.9(4) . . ? 
O16 C15 C4 114.0(4) . . ? 
C15 O16 C17 120.4(4) . . ? 
C15 O16 C17' 104.3(6) . . ? 
O16 C17 C18 105.2(5) . . ? 
C18' C17' O16 103.0(11) . . ? 
C21 O20 Rh1 119.6(2) . . ? 
O22 C21 O20 125.7(3) . . ? 
O22 C21 C23 117.8(3) . . ? 
O20 C21 C23 116.5(3) . . ? 
C21 O22 Rh1 118.5(2) . 2_775 ? 
C31 O30 Rh1 119.7(2) . . ? 
O30 C31 O32 125.6(3) . . ? 
O30 C31 C33 117.3(3) . . ? 
O32 C31 C33 117.1(3) . . ? 
C31 O32 Rh1 118.8(2) . 2_775 ? 
  
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 O15  0.9000(2) 2.032(8) 2.785(4) 140.4(9) . yes 
  
_refine_diff_density_max    0.493 
_refine_diff_density_min   -0.527 
_refine_diff_density_rms    0.073 
  
  
  
#===END

