 
data_39b
  
_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, C6 H5 Cl'
_chemical_formula_sum 
 'C42 H49 Cl N4 O16 Rh2' 
_chemical_formula_weight          1107.12 
  
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' 
 'Cl'  'Cl'   0.3639   0.7018 
 '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                    9.1058(3) 
_cell_length_b                    10.9723(4) 
_cell_length_c                    12.3084(4) 
_cell_angle_alpha                 86.651(3) 
_cell_angle_beta                  88.222(3) 
_cell_angle_gamma                 74.366(3) 
_cell_volume                      1182.09(7) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     173(2) 
_cell_measurement_reflns_used     8897 
_cell_measurement_theta_min       4.1640 
_cell_measurement_theta_max       72.3330 
  
_exptl_crystal_description        tablets 
_exptl_crystal_colour             Purple 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_method     ? 
_exptl_crystal_density_diffrn     1.555 
_exptl_crystal_F_000              564 
_exptl_transmission_factor_min    ? 
_exptl_transmission_factor_max    ? 
_exptl_crystal_size_max           0.155 
_exptl_crystal_size_mid           0.086 
_exptl_crystal_size_min           0.047 
_exptl_absorpt_coefficient_mu     6.785 
_shelx_estimated_absorpt_T_min    ? 
_shelx_estimated_absorpt_T_max    ? 
_exptl_absorpt_correction_type    analytical 
_exptl_absorpt_correction_T_min   0.496 
_exptl_absorpt_correction_T_max   0.782 
_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             25022 
_diffrn_reflns_av_unetI/netI      0.0376 
_diffrn_reflns_av_R_equivalents   0.0563 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -15 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          3.598 
_diffrn_reflns_theta_max          73.764 
_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              4701 
_reflns_number_gt                 3943 
_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)+(0.0558P)²+0.2678P] 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          4701 
_refine_ls_number_parameters      308 
_refine_ls_number_restraints      21 
_refine_ls_R_factor_all           0.0483 
_refine_ls_R_factor_gt            0.0366 
_refine_ls_wR_factor_ref          0.0974 
_refine_ls_wR_factor_gt           0.0901 
_refine_ls_goodness_of_fit_ref    1.055 
_refine_ls_restrained_S_all       1.056 
_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 0.53660(3) 0.39293(2) 0.47134(2) 0.03091(10) Uani 1 1 d . . . . . 
N1 N 0.6170(3) 0.1838(3) 0.4309(2) 0.0290(6) Uani 1 1 d . . . . . 
N2 N 0.5574(3) 0.1094(3) 0.3721(2) 0.0340(6) Uani 1 1 d . . . . . 
C3 C 0.6258(4) -0.0147(3) 0.3949(3) 0.0348(7) Uani 1 1 d . . . . . 
O3 O 0.5817(3) -0.1005(2) 0.3413(2) 0.0441(6) Uani 1 1 d D . . . . 
H3 H 0.6293(15) -0.1807(4) 0.3634(10) 0.11(2) Uiso 1 1 d D . . . . 
C4 C 0.7322(4) -0.0218(3) 0.4752(3) 0.0345(7) Uani 1 1 d . . . . . 
C5 C 0.7213(4) 0.1040(3) 0.4951(3) 0.0363(8) Uani 1 1 d . . . . . 
H5A H 0.779844 0.130147 0.547216 0.044 Uiso 1 1 calc R U . . . 
C6 C 0.4453(4) 0.1625(4) 0.2882(3) 0.0388(8) Uani 1 1 d . . . . . 
H6A H 0.378332 0.243798 0.311955 0.047 Uiso 1 1 calc R U . . . 
H6B H 0.380821 0.103934 0.280436 0.047 Uiso 1 1 calc R U . . . 
C7 C 0.5154(5) 0.1851(4) 0.1786(3) 0.0402(8) Uani 1 1 d . . . . . 
C8 C 0.5261(5) 0.3056(4) 0.1443(3) 0.0459(9) Uani 1 1 d . . . . . 
H8A H 0.491101 0.374005 0.190810 0.055 Uiso 1 1 calc R U . . . 
C9 C 0.5872(5) 0.3263(4) 0.0435(3) 0.0497(10) Uani 1 1 d . . . . . 
H9A H 0.594520 0.408963 0.021471 0.060 Uiso 1 1 calc R U . . . 
C10 C 0.6380(6) 0.2289(4) -0.0262(3) 0.0512(10) Uani 1 1 d . . . . . 
C11 C 0.6336(7) 0.1088(5) 0.0079(4) 0.0694(15) Uani 1 1 d . . . . . 
H11A H 0.671579 0.040284 -0.038120 0.083 Uiso 1 1 calc R U . . . 
C12 C 0.5733(7) 0.0877(4) 0.1098(3) 0.0630(13) Uani 1 1 d . . . . . 
H12A H 0.571786 0.003979 0.133039 0.076 Uiso 1 1 calc R U . . . 
O13 O 0.6912(4) 0.2618(3) -0.1260(2) 0.0651(9) Uani 1 1 d . . . . . 
C14 C 0.7400(9) 0.1649(6) -0.2005(4) 0.087(2) Uani 1 1 d . . . . . 
H14A H 0.767289 0.201421 -0.270312 0.131 Uiso 1 1 calc R U . . . 
H14B H 0.657309 0.125430 -0.211227 0.131 Uiso 1 1 calc R U . . . 
H14C H 0.829065 0.100849 -0.171617 0.131 Uiso 1 1 calc R U . . . 
C15 C 0.8274(4) -0.1388(4) 0.5247(3) 0.0395(8) Uani 1 1 d . . . . . 
O15 O 0.8310(3) -0.2435(2) 0.4973(2) 0.0478(7) Uani 1 1 d . . . . . 
O16 O 0.9084(3) -0.1164(2) 0.6072(2) 0.0439(6) Uani 1 1 d . . . . . 
C17 C 1.0054(5) -0.2264(4) 0.6651(4) 0.0501(10) Uani 1 1 d . . . . . 
H17A H 1.086822 -0.272877 0.615958 0.060 Uiso 1 1 calc R U . . . 
H17B H 0.944658 -0.284505 0.692638 0.060 Uiso 1 1 calc R U . . . 
C18 C 1.0734(6) -0.1802(5) 0.7575(4) 0.0681(13) Uani 1 1 d . . . . . 
H18A H 1.122354 -0.114795 0.730212 0.102 Uiso 1 1 calc R U . . . 
H18B H 1.149627 -0.250951 0.792600 0.102 Uiso 1 1 calc R U . . . 
H18C H 0.993109 -0.144279 0.810460 0.102 Uiso 1 1 calc R U . . . 
O20 O 0.6394(3) 0.4559(2) 0.33836(18) 0.0363(5) Uani 1 1 d . . . . . 
C21 C 0.6335(4) 0.5727(3) 0.3259(3) 0.0352(7) Uani 1 1 d . . . . . 
O22 O 0.5710(3) 0.6572(2) 0.39129(18) 0.0342(5) Uani 1 1 d . . . . . 
C23 C 0.7060(5) 0.6127(4) 0.2233(3) 0.0455(9) Uani 1 1 d . . . . . 
H23A H 0.627570 0.645805 0.168392 0.068 Uiso 1 1 calc R U . . . 
H23B H 0.782488 0.539470 0.195744 0.068 Uiso 1 1 calc R U . . . 
H23C H 0.755258 0.678742 0.238888 0.068 Uiso 1 1 calc R U . . . 
O30 O 0.3359(3) 0.4349(2) 0.39033(19) 0.0354(5) Uani 1 1 d . . . . . 
C31 C 0.2421(4) 0.5420(3) 0.3983(3) 0.0353(7) Uani 1 1 d . . . . . 
O32 O 0.2654(3) 0.6351(2) 0.44640(19) 0.0343(5) Uani 1 1 d . . . . . 
C33 C 0.0901(5) 0.5628(4) 0.3470(3) 0.0491(10) Uani 1 1 d . . . . . 
H33A H 0.045956 0.493168 0.370372 0.074 Uiso 1 1 calc R U . . . 
H33B H 0.102509 0.565709 0.267622 0.074 Uiso 1 1 calc R U . . . 
H33C H 0.022074 0.643162 0.369435 0.074 Uiso 1 1 calc R U . . . 
Cl1 Cl 0.9423(6) 0.8149(5) 0.0556(4) 0.0957(16) Uani 0.353(4) 1 d D U P A -1 
C41 C 0.9611(12) 0.6621(6) 0.0176(9) 0.060(3) Uiso 0.353(4) 1 d DG U P A -1 
C42 C 1.0849(10) 0.5667(9) 0.0562(10) 0.059(4) Uiso 0.353(4) 1 d DG U P A -1 
H42A H 1.161519 0.587317 0.096402 0.071 Uiso 0.353(4) 1 calc R U P A -1 
C43 C 1.0965(10) 0.4411(7) 0.0361(9) 0.066(4) Uiso 0.353(4) 1 d G U P A -1 
H43A H 1.181029 0.375836 0.062562 0.079 Uiso 0.353(4) 1 calc R U P A -1 
C44 C 0.9843(14) 0.4109(6) -0.0226(11) 0.064(4) Uiso 0.353(4) 1 d G U P A -1 
H44A H 0.992211 0.325033 -0.036374 0.076 Uiso 0.353(4) 1 calc R U P A -1 
C45 C 0.8605(13) 0.5063(9) -0.0613(11) 0.075(5) Uiso 0.353(4) 1 d G U P A -1 
H45A H 0.783880 0.485709 -0.101470 0.090 Uiso 0.353(4) 1 calc R U P A -1 
C46 C 0.8489(10) 0.6320(8) -0.0412(9) 0.065(4) Uiso 0.353(4) 1 d DG U P A -1 
H46A H 0.764367 0.697191 -0.067632 0.078 Uiso 0.353(4) 1 calc R U P A -1 
Cl1' Cl 0.8161(15) 0.7473(12) -0.0371(12) 0.114(4) Uiso 0.147(4) 1 d D U P A -2 
C41' C 0.935(2) 0.5935(12) -0.014(2) 0.063(7) Uiso 0.147(4) 1 d DG U P A -2 
C42' C 0.891(3) 0.4910(15) -0.050(2) 0.050(8) Uiso 0.147(4) 1 d DG U P A -2 
H42B H 0.798690 0.504707 -0.088528 0.060 Uiso 0.147(4) 1 calc R U P A -2 
C43' C 0.983(3) 0.3685(13) -0.030(3) 0.073(9) Uiso 0.147(4) 1 d G U P A -2 
H43B H 0.952376 0.298426 -0.054457 0.087 Uiso 0.147(4) 1 calc R U P A -2 
C44' C 1.118(3) 0.3485(15) 0.026(3) 0.090(12) Uiso 0.147(4) 1 d G U P A -2 
H44B H 1.180274 0.264706 0.039829 0.109 Uiso 0.147(4) 1 calc R U P A -2 
C45' C 1.162(3) 0.451(2) 0.062(3) 0.059(8) Uiso 0.147(4) 1 d G U P A -2 
H45B H 1.254488 0.437268 0.100044 0.070 Uiso 0.147(4) 1 calc R U P A -2 
C46' C 1.071(2) 0.5735(17) 0.042(2) 0.070(13) Uiso 0.147(4) 1 d DG U P A -2 
H46B H 1.100803 0.643551 0.065974 0.084 Uiso 0.147(4) 1 calc R U P A -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 
Rh1 O32 2.037(2) 2_666 ? 
Rh1 O30 2.037(2) . ? 
Rh1 O20 2.038(2) . ? 
Rh1 O22 2.049(2) 2_666 ? 
Rh1 N1 2.292(3) . ? 
Rh1 Rh1 2.4049(5) 2_666 ? 
N1 C5 1.345(5) . ? 
N1 N2 1.349(4) . ? 
N2 C3 1.353(5) . ? 
N2 C6 1.457(4) . ? 
C3 O3 1.332(4) . ? 
C3 C4 1.390(5) . ? 
C4 C5 1.393(5) . ? 
C4 C15 1.452(5) . ? 
C6 C7 1.510(5) . ? 
C7 C12 1.383(6) . ? 
C7 C8 1.392(5) . ? 
C8 C9 1.376(6) . ? 
C9 C10 1.382(6) . ? 
C10 C11 1.370(6) . ? 
C10 O13 1.371(5) . ? 
C11 C12 1.385(6) . ? 
O13 C14 1.415(6) . ? 
C15 O15 1.208(5) . ? 
C15 O16 1.345(5) . ? 
O16 C17 1.453(5) . ? 
C17 C18 1.488(6) . ? 
O20 C21 1.269(4) . ? 
C21 O22 1.268(4) . ? 
C21 C23 1.504(5) . ? 
O30 C31 1.260(4) . ? 
C31 O32 1.278(4) . ? 
C31 C33 1.495(5) . ? 
Cl1 C41 1.729(8) . ? 
C41 C42 1.3900 . ? 
C41 C46 1.3900 . ? 
C42 C43 1.3900 . ? 
C43 C44 1.3900 . ? 
C44 C45 1.3900 . ? 
C45 C46 1.3900 . ? 
Cl1' C41' 1.755(13) . ? 
C41' C42' 1.3900 . ? 
C41' C46' 1.3900 . ? 
C42' C43' 1.3900 . ? 
C43' C44' 1.3900 . ? 
C44' C45' 1.3900 . ? 
C45' C46' 1.3900 . ? 
  
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 O30 175.78(9) 2_666 . ? 
O32 Rh1 O20 88.85(10) 2_666 . ? 
O30 Rh1 O20 90.05(10) . . ? 
O32 Rh1 O22 90.95(9) 2_666 2_666 ? 
O30 Rh1 O22 89.84(10) . 2_666 ? 
O20 Rh1 O22 175.84(9) . 2_666 ? 
O32 Rh1 N1 87.35(10) 2_666 . ? 
O30 Rh1 N1 96.80(9) . . ? 
O20 Rh1 N1 94.66(9) . . ? 
O22 Rh1 N1 89.48(9) 2_666 . ? 
O32 Rh1 Rh1 88.47(7) 2_666 2_666 ? 
O30 Rh1 Rh1 87.42(7) . 2_666 ? 
O20 Rh1 Rh1 88.00(7) . 2_666 ? 
O22 Rh1 Rh1 87.85(7) 2_666 2_666 ? 
N1 Rh1 Rh1 175.00(7) . 2_666 ? 
C5 N1 N2 105.6(3) . . ? 
C5 N1 Rh1 118.5(2) . . ? 
N2 N1 Rh1 133.4(2) . . ? 
N1 N2 C3 111.1(3) . . ? 
N1 N2 C6 121.6(3) . . ? 
C3 N2 C6 127.0(3) . . ? 
O3 C3 N2 118.3(3) . . ? 
O3 C3 C4 134.1(3) . . ? 
N2 C3 C4 107.6(3) . . ? 
C3 C4 C5 104.4(3) . . ? 
C3 C4 C15 124.9(3) . . ? 
C5 C4 C15 130.6(3) . . ? 
N1 C5 C4 111.2(3) . . ? 
N2 C6 C7 113.6(3) . . ? 
C12 C7 C8 117.6(4) . . ? 
C12 C7 C6 121.7(3) . . ? 
C8 C7 C6 120.7(4) . . ? 
C9 C8 C7 120.5(4) . . ? 
C8 C9 C10 121.0(4) . . ? 
C11 C10 O13 124.9(4) . . ? 
C11 C10 C9 119.2(4) . . ? 
O13 C10 C9 115.8(4) . . ? 
C10 C11 C12 119.7(4) . . ? 
C7 C12 C11 121.9(4) . . ? 
C10 O13 C14 117.3(4) . . ? 
O15 C15 O16 123.9(4) . . ? 
O15 C15 C4 124.5(4) . . ? 
O16 C15 C4 111.6(3) . . ? 
C15 O16 C17 116.8(3) . . ? 
O16 C17 C18 107.5(4) . . ? 
C21 O20 Rh1 119.4(2) . . ? 
O22 C21 O20 125.7(3) . . ? 
O22 C21 C23 118.1(3) . . ? 
O20 C21 C23 116.2(3) . . ? 
C21 O22 Rh1 119.0(2) . 2_666 ? 
C31 O30 Rh1 119.8(2) . . ? 
O30 C31 O32 125.7(3) . . ? 
O30 C31 C33 117.5(3) . . ? 
O32 C31 C33 116.8(3) . . ? 
C31 O32 Rh1 118.3(2) . 2_666 ? 
C42 C41 C46 120.0 . . ? 
C42 C41 Cl1 118.2(5) . . ? 
C46 C41 Cl1 121.5(6) . . ? 
C41 C42 C43 120.0 . . ? 
C44 C43 C42 120.0 . . ? 
C43 C44 C45 120.0 . . ? 
C46 C45 C44 120.0 . . ? 
C45 C46 C41 120.0 . . ? 
C42' C41' C46' 120.0 . . ? 
C42' C41' Cl1' 119.5(7) . . ? 
C46' C41' Cl1' 120.5(7) . . ? 
C43' C42' C41' 120.0 . . ? 
C42' C43' C44' 120.0 . . ? 
C45' C44' C43' 120.0 . . ? 
C44' C45' C46' 120.0 . . ? 
C45' C46' C41' 120.0 . . ? 
  
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(1) 2.436(10) 3.049(4) 125.6(9) . yes 
O3 H3 O22  0.9000(1) 1.997(10) 2.720(3) 136.3(12) 1_545 yes 
  
_refine_diff_density_max    1.006 
_refine_diff_density_min   -0.454 
_refine_diff_density_rms    0.091 
  
  
  
#===END

