#------------------------------------------------------------------------------
#$Date: 2019-11-25 15:25:19 +0200 (Mon, 25 Nov 2019) $
#$Revision: 241193 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/08/4130833.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_4130833
loop_
_publ_author_name
'Nakamura, Munechika'
'Kishimoto, Kazuki'
'Kobori, Yasuhiro'
'Abe, Tomoka'
'Yoza, Kenji'
'Kobayashi, Kenji'
_publ_section_title
;
 Self-Assembled Molecular Gear: A 4:1 Complex of Rh(III)Cl
 Tetraarylporphyrin and Tetra(p-pyridyl)cavitand.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12564
_journal_page_last               12577
_journal_paper_doi               10.1021/jacs.6b07284
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C67.5 H55.5 Cl8.5 N5 O3.25 Rh'
_chemical_formula_weight         1392.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0036(9)
_cell_length_b                   25.0036(9)
_cell_length_c                   23.9683(8)
_cell_measurement_temperature    100
_cell_volume                     14984.5(9)
_computing_cell_refinement       'APEX2 v2014.9 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service V4.2.2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS Inc., 2004)'
_computing_publication_material
'Generate Report V2014.1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51713
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'micro focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             5688
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 4612 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         13248
_refine_ls_number_restraints     1507
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0837
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1569P)²+91.5361P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2459
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11021
_reflns_number_total             13248
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja6b07284_si_002.cif
_cod_data_source_block           b
_cod_original_cell_volume        14984.5(12)
_cod_original_formula_sum        'C67.50 H55.50 Cl8.50 N5 O3.25 Rh'
_cod_database_code               4130833
_shelx_shelxl_version_number     2014/7
_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.
;
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.961
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
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
C1 C 0.3240(5) 0.4926(5) 0.4447(5) 0.034(2) Uani 1 1 d . U . . .
H1A H 0.3603 0.4956 0.4611 0.041 Uiso 1 1 calc R U . . .
H1B H 0.2982 0.4910 0.4760 0.041 Uiso 1 1 calc R U . . .
C2 C 0.3577(4) 0.6748(4) 0.5544(5) 0.028(2) Uani 1 1 d . U . . .
H2 H 0.3770 0.6814 0.5878 0.034 Uiso 1 1 calc R U . . .
C3 C 0.3389(5) 0.7170(5) 0.7035(5) 0.032(2) Uani 1 1 d . U . . .
C4 C 0.4451(5) 0.6147(5) 0.3403(5) 0.032(2) Uani 1 1 d . U . . .
C5 C 0.2823(6) 0.6584(6) 0.7420(6) 0.041(3) Uani 1 1 d . U . . .
H5 H 0.2666 0.6316 0.7648 0.049 Uiso 1 1 calc R U . . .
C6 C 0.2950(5) 0.8446(5) 0.4456(5) 0.038(2) Uani 1 1 d . U . . .
H6 H 0.3147 0.8595 0.4154 0.046 Uiso 1 1 calc R U . . .
C7 C 0.2808(4) 0.6842(4) 0.5027(5) 0.028(2) Uani 1 1 d . U . . .
H7 H 0.2452 0.6972 0.4990 0.034 Uiso 1 1 calc R U . . .
C8 C 0.3809(5) 0.6432(4) 0.5136(5) 0.030(2) Uani 1 1 d . U . . .
H8 H 0.4152 0.6278 0.5195 0.036 Uiso 1 1 calc R U . . .
C9 C 0.3165(5) 0.8220(5) 0.4955(5) 0.033(2) Uani 1 1 d . U . . .
C10 C 0.1257(5) 0.7015(5) 0.6176(5) 0.034(2) Uani 1 1 d . U . . .
H10 H 0.0992 0.6798 0.6347 0.041 Uiso 1 1 calc R U . . .
C11 C 0.3021(5) 0.6530(5) 0.4604(5) 0.031(2) Uani 1 1 d . U . . .
H11 H 0.2811 0.6445 0.4287 0.037 Uiso 1 1 calc R U . . .
C12 C 0.3802(4) 0.6083(4) 0.4150(5) 0.029(2) Uani 1 1 d . U . . .
C13 C 0.3540(4) 0.6342(4) 0.4642(5) 0.028(2) Uani 1 1 d . U . . .
C14 C 0.3556(5) 0.4932(5) 0.3139(5) 0.033(2) Uani 1 1 d . U . . .
H14 H 0.3173 0.4911 0.3257 0.040 Uiso 1 1 calc R U . . .
C15 C 0.3583(4) 0.5640(4) 0.3893(5) 0.030(2) Uani 1 1 d . U . . .
C16 C 0.2055(4) 0.6746(4) 0.6749(5) 0.030(2) Uani 1 1 d . U . . .
C17 C 0.2278(5) 0.8120(4) 0.5014(5) 0.031(2) Uani 1 1 d . U . . .
C18 C 0.3975(5) 0.7734(5) 0.6453(5) 0.036(2) Uani 1 1 d . U . . .
C19 C 0.1177(5) 0.7374(5) 0.5769(5) 0.034(2) Uani 1 1 d . U . . .
H19 H 0.0841 0.7464 0.5608 0.041 Uiso 1 1 calc R U . . .
C20 C 0.4447(5) 0.8138(5) 0.5769(6) 0.042(3) Uani 1 1 d . U . . .
H20 H 0.4725 0.8295 0.5554 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4251(4) 0.6333(4) 0.3903(5) 0.027(2) Uani 1 1 d . U . . .
C22 C 0.3791(5) 0.5436(5) 0.3391(5) 0.031(2) Uani 1 1 d . U . . .
C23 C 0.1684(5) 0.7596(5) 0.5619(5) 0.033(2) Uani 1 1 d . U . . .
C24 C 0.3570(6) 0.4919(6) 0.2488(5) 0.047(3) Uani 1 1 d . U . . .
H23A H 0.3947 0.4946 0.2365 0.057 Uiso 0.451(9) 1 calc R U P A 1
H23B H 0.3431 0.4569 0.2361 0.057 Uiso 0.451(9) 1 calc R U P A 1
H23C H 0.3945 0.4915 0.2355 0.057 Uiso 0.549(9) 1 calc R U P A 2
H23D H 0.3391 0.5240 0.2335 0.057 Uiso 0.549(9) 1 calc R U P A 2
C25 C 0.4496(5) 0.7947(6) 0.6288(6) 0.042(3) Uani 1 1 d . U . . .
H25 H 0.4811 0.7949 0.6509 0.050 Uiso 1 1 calc R U . . .
C26 C 0.4226(4) 0.5699(5) 0.3154(5) 0.030(2) Uani 1 1 d . U . . .
H26 H 0.4372 0.5569 0.2814 0.036 Uiso 1 1 calc R U . . .
C27 C 0.3910(5) 0.8066(5) 0.5595(5) 0.034(2) Uani 1 1 d . U . . .
C28 C 0.2587(5) 0.6819(5) 0.6929(5) 0.031(2) Uani 1 1 d . U . . .
C29 C 0.1823(4) 0.7020(4) 0.6307(5) 0.029(2) Uani 1 1 d . U . . .
C30 C 0.3305(5) 0.6810(5) 0.7497(5) 0.037(2) Uani 1 1 d . U . . .
H30 H 0.3544 0.6746 0.7797 0.045 Uiso 1 1 calc R U . . .
C31 C 0.3859(5) 0.7452(5) 0.6936(5) 0.039(2) Uani 1 1 d . U . . .
C32 C 0.3704(5) 0.8222(5) 0.5087(5) 0.034(2) Uani 1 1 d . U . . .
C33 C 0.2391(5) 0.8406(5) 0.4498(5) 0.035(2) Uani 1 1 d . U . . .
H33 H 0.2136 0.8541 0.4240 0.042 Uiso 1 1 calc R U . . .
C34 C 0.1787(5) 0.7954(5) 0.5179(5) 0.038(2) Uani 1 1 d . U . . .
C1A C 0.5091(5) 0.7046(6) 0.7754(6) 0.093(5) Uani 1 1 d G U . . .
H1A1 H 0.5360 0.6778 0.7746 0.112 Uiso 1 1 calc R U . . .
C2A C 0.4679(5) 0.7036(5) 0.7365(5) 0.075(4) Uani 1 1 d G U . . .
H2A H 0.4666 0.6761 0.7091 0.090 Uiso 1 1 calc R U . . .
C3A C 0.4285(4) 0.7428(5) 0.7376(4) 0.054(3) Uani 1 1 d G U . . .
C4A C 0.4303(5) 0.7830(4) 0.7776(5) 0.080(4) Uani 1 1 d G U . . .
H4A H 0.4033 0.8098 0.7783 0.096 Uiso 1 1 calc R U . . .
C5A C 0.4715(6) 0.7840(5) 0.8165(5) 0.094(5) Uani 1 1 d G U . . .
H5A H 0.4727 0.8114 0.8438 0.113 Uiso 1 1 calc R U . . .
C6A C 0.5109(5) 0.7448(6) 0.8154(5) 0.093(4) Uani 1 1 d G U . . .
C7A C 0.5556(10) 0.7445(13) 0.8585(10) 0.115(7) Uani 1 1 d . U . . .
H7A1 H 0.5836 0.7698 0.8473 0.173 Uiso 1 1 calc R U . . .
H7A2 H 0.5709 0.7085 0.8612 0.173 Uiso 1 1 calc R U . . .
H7A3 H 0.5412 0.7550 0.8949 0.173 Uiso 1 1 calc R U . . .
C1B C 0.4652(4) 0.8196(3) 0.3862(4) 0.057(3) Uani 1 1 d G U . . .
H1B1 H 0.4768 0.7945 0.3590 0.069 Uiso 1 1 calc R U . . .
C2B C 0.4266(4) 0.8050(3) 0.4251(4) 0.046(3) Uani 1 1 d G U . . .
H2B H 0.4119 0.7700 0.4245 0.055 Uiso 1 1 calc R U . . .
C3B C 0.4096(3) 0.8416(3) 0.4649(3) 0.039(2) Uani 1 1 d G U . . .
C4B C 0.4311(4) 0.8929(3) 0.4658(3) 0.049(3) Uani 1 1 d G U . . .
H4B H 0.4195 0.9179 0.4930 0.058 Uiso 1 1 calc R U . . .
C5B C 0.4697(4) 0.9075(3) 0.4269(4) 0.057(3) Uani 1 1 d G U . . .
H5B H 0.4844 0.9425 0.4275 0.068 Uiso 1 1 calc R U . . .
C6B C 0.4867(4) 0.8708(4) 0.3871(4) 0.061(3) Uani 1 1 d G U . . .
C7B C 0.5300(8) 0.8871(9) 0.3461(9) 0.085(5) Uani 1 1 d . U . . .
H7B1 H 0.5287 0.9258 0.3403 0.127 Uiso 1 1 calc R U . . .
H7B2 H 0.5242 0.8687 0.3105 0.127 Uiso 1 1 calc R U . . .
H7B3 H 0.5651 0.8771 0.3611 0.127 Uiso 1 1 calc R U . . .
C1C C 0.0747(4) 0.8270(4) 0.4054(3) 0.061(3) Uani 1 1 d G U . . .
H1C H 0.0670 0.8178 0.3678 0.074 Uiso 1 1 calc R U . . .
C2C C 0.1182(4) 0.8039(4) 0.4324(4) 0.050(3) Uani 1 1 d G U . . .
H2C H 0.1402 0.7789 0.4132 0.060 Uiso 1 1 calc R U . . .
C3C C 0.1295(3) 0.8173(4) 0.4874(4) 0.044(3) Uani 1 1 d G U . . .
C4C C 0.0974(4) 0.8538(4) 0.5155(3) 0.064(4) Uani 1 1 d G U . . .
H4C H 0.1051 0.8629 0.5531 0.077 Uiso 1 1 calc R U . . .
C5C C 0.0539(4) 0.8769(4) 0.4886(5) 0.076(4) Uani 1 1 d G U . . .
H5C H 0.0319 0.9018 0.5078 0.091 Uiso 1 1 calc R U . . .
C6C C 0.0426(4) 0.8635(5) 0.4335(5) 0.072(4) Uani 1 1 d G U . . .
C7C C -0.0045(9) 0.8887(9) 0.4043(10) 0.089(6) Uani 1 1 d . U . . .
H7C1 H -0.0351 0.8899 0.4298 0.134 Uiso 1 1 calc R U . . .
H7C2 H -0.0139 0.8674 0.3714 0.134 Uiso 1 1 calc R U . . .
H7C3 H 0.0048 0.9251 0.3927 0.134 Uiso 1 1 calc R U . . .
C1D C 0.1275(4) 0.5495(3) 0.7091(4) 0.054(3) Uani 1 1 d G U . . .
H1D H 0.1178 0.5170 0.6913 0.064 Uiso 1 1 calc R U . . .
C2D C 0.1570(4) 0.5877(3) 0.6803(3) 0.044(3) Uani 1 1 d G U . . .
H2D H 0.1673 0.5814 0.6428 0.053 Uiso 1 1 calc R U . . .
C3D C 0.1713(3) 0.6352(3) 0.7065(3) 0.034(2) Uani 1 1 d G U . . .
C4D C 0.1562(3) 0.6445(3) 0.7614(3) 0.038(2) Uani 1 1 d G U . . .
H4D H 0.1660 0.6770 0.7793 0.045 Uiso 1 1 calc R U . . .
C5D C 0.1268(3) 0.6063(3) 0.7903(3) 0.045(3) Uani 1 1 d G U . . .
H5D H 0.1165 0.6126 0.8278 0.054 Uiso 1 1 calc R U . . .
C6D C 0.1124(4) 0.5588(3) 0.7641(4) 0.050(3) Uani 1 1 d G U . . .
C7D C 0.0801(6) 0.5157(6) 0.7957(7) 0.064(4) Uani 1 1 d . U . . .
H7D1 H 0.1022 0.5002 0.8253 0.096 Uiso 1 1 calc R U . . .
H7D2 H 0.0692 0.4876 0.7696 0.096 Uiso 1 1 calc R U . . .
H7D3 H 0.0482 0.5321 0.8122 0.096 Uiso 1 1 calc R U . . .
C1E C 0.3247(13) 0.5364(13) 0.2204(13) 0.049(5) Uani 0.451(9) 1 d . U P A 1
H1E H 0.3314 0.5709 0.2403 0.058 Uiso 0.451(9) 1 calc R U P A 1
C2E C 0.2671(14) 0.5251(15) 0.2209(17) 0.064(8) Uani 0.451(9) 1 d . U P A 1
H2E1 H 0.2613 0.4867 0.2150 0.096 Uiso 0.451(9) 1 calc R U P A 1
H2E2 H 0.2496 0.5453 0.1910 0.096 Uiso 0.451(9) 1 calc R U P A 1
H2E3 H 0.2520 0.5357 0.2570 0.096 Uiso 0.451(9) 1 calc R U P A 1
C3E C 0.3375(16) 0.5436(16) 0.1586(14) 0.062(7) Uani 0.451(9) 1 d . U P A 1
H3E1 H 0.3667 0.5194 0.1481 0.093 Uiso 0.451(9) 1 calc R U P A 1
H3E2 H 0.3484 0.5807 0.1518 0.093 Uiso 0.451(9) 1 calc R U P A 1
H3E3 H 0.3057 0.5353 0.1364 0.093 Uiso 0.451(9) 1 calc R U P A 1
C1F C 0.3269(13) 0.4396(14) 0.2293(13) 0.067(5) Uani 0.549(9) 1 d . U P A 2
H1F H 0.3440 0.4091 0.2496 0.081 Uiso 0.549(9) 1 calc R U P A 2
C2F C 0.2671(14) 0.4376(16) 0.2435(14) 0.079(8) Uani 0.549(9) 1 d . U P A 2
H2F1 H 0.2604 0.4081 0.2695 0.119 Uiso 0.549(9) 1 calc R U P A 2
H2F2 H 0.2464 0.4320 0.2093 0.119 Uiso 0.549(9) 1 calc R U P A 2
H2F3 H 0.2564 0.4715 0.2609 0.119 Uiso 0.549(9) 1 calc R U P A 2
C3F C 0.3393(18) 0.430(2) 0.1628(17) 0.097(9) Uani 0.549(9) 1 d . U P A 2
H3F1 H 0.3478 0.4643 0.1451 0.145 Uiso 0.549(9) 1 calc R U P A 2
H3F2 H 0.3078 0.4144 0.1448 0.145 Uiso 0.549(9) 1 calc R U P A 2
H3F3 H 0.3697 0.4056 0.1588 0.145 Uiso 0.549(9) 1 calc R U P A 2
C1M C 0.2605(6) 0.6969(6) 0.2948(9) 0.112(5) Uani 0.739(8) 1 d D U P B 1
H1M H 0.2443 0.7109 0.2595 0.134 Uiso 0.739(8) 1 calc R U P B 1
C1R C 0.2481(9) 0.6787(10) 0.2945(14) 0.119(6) Uani 0.261(8) 1 d D U P B 2
H1R H 0.2399 0.6899 0.2553 0.143 Uiso 0.261(8) 1 calc R U P B 2
C1N C 0.0830(6) 0.6090(11) 0.5071(8) 0.116(5) Uani 0.67(4) 1 d D U P A 1
H1N H 0.0759 0.6421 0.5294 0.139 Uiso 0.67(4) 1 calc R U P A 1
C1P C 0.1445(6) 0.6149(9) 0.5149(10) 0.116(6) Uani 0.33(4) 1 d D U P A 2
H1P H 0.1563 0.6400 0.5450 0.140 Uiso 0.33(4) 1 calc R U P A 2
C1Q C 0.3889(11) 0.9565(6) 0.6551(9) 0.117(7) Uani 0.5 1 d D U P . .
H1Q H 0.3565 0.9527 0.6310 0.141 Uiso 0.5 1 calc R U P . .
Cl02 Cl 0.25998(13) 0.83321(12) 0.65267(13) 0.0397(7) Uani 1 1 d . U . . .
Cl1M Cl 0.2528(4) 0.7436(3) 0.3478(4) 0.096(2) Uani 0.739(8) 1 d D U P B 1
Cl2M Cl 0.2317(5) 0.6357(4) 0.3117(4) 0.129(3) Uani 0.739(8) 1 d D U P B 1
Cl3M Cl 0.3289(3) 0.6867(3) 0.2854(4) 0.120(3) Uani 0.739(8) 1 d D U P B 1
Cl1N Cl 0.0640(6) 0.5536(7) 0.5460(6) 0.126(5) Uani 0.451(9) 1 d D U P A 1
Cl2N Cl 0.0459(6) 0.6115(6) 0.4464(5) 0.115(5) Uani 0.451(9) 1 d D U P A 1
Cl3N Cl 0.1510(5) 0.6046(7) 0.4935(7) 0.121(4) Uani 0.451(9) 1 d D U P A 1
Cl1P Cl 0.0890(4) 0.5793(5) 0.5373(5) 0.100(3) Uani 0.549(9) 1 d D U P A 2
Cl2P Cl 0.1306(5) 0.6510(5) 0.4547(5) 0.116(4) Uani 0.549(9) 1 d D U P A 2
Cl3P Cl 0.1954(4) 0.5701(5) 0.5001(6) 0.128(4) Uani 0.549(9) 1 d D U P A 2
Cl1Q Cl 0.4451(7) 0.9564(6) 0.6131(6) 0.142(5) Uani 0.5 1 d D U P . .
Cl2Q Cl 0.3907(4) 0.9038(3) 0.7016(5) 0.095(3) Uani 0.5 1 d D U P . .
Cl3Q Cl 0.3847(7) 1.0164(4) 0.6913(6) 0.127(4) Uani 0.5 1 d D U P . .
Cl1R Cl 0.3050(10) 0.7115(11) 0.3177(13) 0.128(6) Uani 0.261(8) 1 d D U P B 2
Cl2R Cl 0.2590(11) 0.6100(9) 0.2969(12) 0.116(7) Uani 0.261(8) 1 d D U P B 2
Cl3R Cl 0.1944(9) 0.6940(11) 0.3376(12) 0.126(6) Uani 0.261(8) 1 d D U P B 2
N21 N 0.2072(3) 0.7374(3) 0.5959(7) 0.0287(17) Uani 1 1 d . U . . .
N22 N 0.3629(3) 0.7823(3) 0.6019(5) 0.0307(17) Uani 1 1 d . U . . .
N23 N 0.3087(4) 0.6965(4) 0.5484(4) 0.0274(19) Uani 1 1 d . U . . .
N00I N 0.2761(4) 0.8014(4) 0.5267(4) 0.031(2) Uani 1 1 d . U . . .
N00K N 0.2949(4) 0.7167(4) 0.6697(4) 0.0287(19) Uani 1 1 d . U . . .
O004 O 0.4443(3) 0.6791(3) 0.4146(3) 0.0335(17) Uani 1 1 d . U . . .
O006 O 0.3134(3) 0.5398(3) 0.4126(3) 0.0350(17) Uani 1 1 d . U . . .
O1W O 0.5000 0.5000 0.1846(7) 0.050(4) Uani 1 4 d S TU P . .
O2W O 0.5000 0.5000 0.4412(15) 0.113(9) Uani 1 4 d S TU P . .
O3W O 0.0000 0.0000 0.5632(18) 0.149(14) Uani 1 4 d S TU P . .
O4W O 0.5452(16) 0.6840(16) 0.603(2) 0.142(12) Uani 0.5 1 d . U P . .
Rh01 Rh 0.28513(3) 0.75950(3) 0.59880(6) 0.0245(2) Uani 1 1 d . U . . .
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'
Cl Cl 0.1484 0.1585 '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
O004 C1 O006 114.8(9) 3_655 .
O004 C1 H1A 108.6 3_655 .
O006 C1 H1A 108.6 . .
O004 C1 H1B 108.6 3_655 .
O006 C1 H1B 108.6 . .
H1A C1 H1B 107.5 . .
N23 C2 C8 122.4(10) . .
N23 C2 H2 118.8 . .
C8 C2 H2 118.8 . .
N00K C3 C31 125.6(11) . .
N00K C3 C30 109.5(10) . .
C31 C3 C30 124.8(11) . .
C21 C4 C26 119.9(11) . .
C21 C4 C14 118.3(10) . 4_565
C26 C4 C14 121.8(11) . 4_565
C30 C5 C28 108.0(11) . .
C30 C5 H5 126.0 . .
C28 C5 H5 126.0 . .
C33 C6 C9 106.6(11) . .
C33 C6 H6 126.7 . .
C9 C6 H6 126.7 . .
N23 C7 C11 121.8(10) . .
N23 C7 H7 119.1 . .
C11 C7 H7 119.1 . .
C13 C8 C2 119.6(10) . .
C13 C8 H8 120.2 . .
C2 C8 H8 120.2 . .
N00I C9 C32 126.9(11) . .
N00I C9 C6 109.3(10) . .
C32 C9 C6 123.8(11) . .
C19 C10 C29 107.4(10) . .
C19 C10 H10 126.3 . .
C29 C10 H10 126.3 . .
C13 C11 C7 120.3(11) . .
C13 C11 H11 119.8 . .
C7 C11 H11 119.8 . .
C15 C12 C21 118.7(10) . .
C15 C12 C13 121.8(10) . .
C21 C12 C13 119.1(10) . .
C8 C13 C11 117.3(10) . .
C8 C13 C12 122.3(10) . .
C11 C13 C12 120.3(10) . .
C22 C14 C4 107.3(9) . 3_655
C22 C14 C24 114.1(11) . .
C4 C14 C24 112.4(10) 3_655 .
C22 C14 H14 107.6 . .
C4 C14 H14 107.6 3_655 .
C24 C14 H14 107.6 . .
C12 C15 O006 119.3(10) . .
C12 C15 C22 121.7(11) . .
O006 C15 C22 119.0(10) . .
C29 C16 C28 124.3(10) . .
C29 C16 C3D 117.9(10) . .
C28 C16 C3D 117.8(10) . .
C34 C17 N00I 127.5(11) . .
C34 C17 C33 125.0(11) . .
N00I C17 C33 107.2(10) . .
N22 C18 C31 125.7(11) . .
N22 C18 C25 107.3(10) . .
C31 C18 C25 126.8(12) . .
C10 C19 C23 108.0(11) . .
C10 C19 H19 126.0 . .
C23 C19 H19 126.0 . .
C25 C20 C27 108.3(12) . .
C25 C20 H20 125.9 . .
C27 C20 H20 125.9 . .
O004 C21 C4 121.6(10) . .
O004 C21 C12 117.9(10) . .
C4 C21 C12 120.2(10) . .
C26 C22 C15 117.9(11) . .
C26 C22 C14 122.1(11) . .
C15 C22 C14 119.9(11) . .
N21 C23 C34 124.6(11) . .
N21 C23 C19 108.5(10) . .
C34 C23 C19 126.7(11) . .
C1E C24 C14 114.7(16) . .
C14 C24 C1F 107.7(16) . .
C1E C24 H23A 108.6 . .
C14 C24 H23A 108.6 . .
C1E C24 H23B 108.6 . .
C14 C24 H23B 108.6 . .
H23A C24 H23B 107.6 . .
C14 C24 H23C 110.2 . .
C1F C24 H23C 110.2 . .
C14 C24 H23D 110.2 . .
C1F C24 H23D 110.2 . .
H23C C24 H23D 108.5 . .
C20 C25 C18 107.6(12) . .
C20 C25 H25 126.2 . .
C18 C25 H25 126.2 . .
C4 C26 C22 121.4(11) . .
C4 C26 H26 119.3 . .
C22 C26 H26 119.3 . .
N22 C27 C32 125.8(11) . .
N22 C27 C20 108.9(10) . .
C32 C27 C20 125.3(11) . .
N00K C28 C16 125.4(10) . .
N00K C28 C5 108.6(10) . .
C16 C28 C5 125.7(11) . .
N21 C29 C16 126.6(11) . .
N21 C29 C10 108.5(10) . .
C16 C29 C10 124.6(10) . .
C5 C30 C3 106.7(11) . .
C5 C30 H30 126.6 . .
C3 C30 H30 126.6 . .
C18 C31 C3 125.3(11) . .
C18 C31 C3A 117.3(11) . .
C3 C31 C3A 117.3(11) . .
C27 C32 C9 124.4(11) . .
C27 C32 C3B 117.5(10) . .
C9 C32 C3B 118.1(10) . .
C6 C33 C17 106.9(10) . .
C6 C33 H33 126.5 . .
C17 C33 H33 126.5 . .
C17 C34 C23 125.3(11) . .
C17 C34 C3C 118.7(11) . .
C23 C34 C3C 115.9(10) . .
C2A C1A C6A 120.0 . .
C2A C1A H1A1 120.0 . .
C6A C1A H1A1 120.0 . .
C1A C2A C3A 120.0 . .
C1A C2A H2A 120.0 . .
C3A C2A H2A 120.0 . .
C4A C3A C2A 120.0 . .
C4A C3A C31 118.6(9) . .
C2A C3A C31 121.3(9) . .
C3A C4A C5A 120.0 . .
C3A C4A H4A 120.0 . .
C5A C4A H4A 120.0 . .
C6A C5A C4A 120.0 . .
C6A C5A H5A 120.0 . .
C4A C5A H5A 120.0 . .
C5A C6A C1A 120.0 . .
C5A C6A C7A 120.7(16) . .
C1A C6A C7A 119.3(16) . .
C6A C7A H7A1 109.5 . .
C6A C7A H7A2 109.5 . .
H7A1 C7A H7A2 109.5 . .
C6A C7A H7A3 109.5 . .
H7A1 C7A H7A3 109.5 . .
H7A2 C7A H7A3 109.5 . .
C2B C1B C6B 120.0 . .
C2B C1B H1B1 120.0 . .
C6B C1B H1B1 120.0 . .
C3B C2B C1B 120.0 . .
C3B C2B H2B 120.0 . .
C1B C2B H2B 120.0 . .
C4B C3B C2B 120.0 . .
C4B C3B C32 122.3(7) . .
C2B C3B C32 117.6(7) . .
C3B C4B C5B 120.0 . .
C3B C4B H4B 120.0 . .
C5B C4B H4B 120.0 . .
C4B C5B C6B 120.0 . .
C4B C5B H5B 120.0 . .
C6B C5B H5B 120.0 . .
C5B C6B C1B 120.0 . .
C5B C6B C7B 119.1(11) . .
C1B C6B C7B 120.9(11) . .
C6B C7B H7B1 109.5 . .
C6B C7B H7B2 109.5 . .
H7B1 C7B H7B2 109.5 . .
C6B C7B H7B3 109.5 . .
H7B1 C7B H7B3 109.5 . .
H7B2 C7B H7B3 109.5 . .
C2C C1C C6C 120.0 . .
C2C C1C H1C 120.0 . .
C6C C1C H1C 120.0 . .
C1C C2C C3C 120.0 . .
C1C C2C H2C 120.0 . .
C3C C2C H2C 120.0 . .
C4C C3C C2C 120.0 . .
C4C C3C C34 117.8(8) . .
C2C C3C C34 122.1(8) . .
C5C C4C C3C 120.0 . .
C5C C4C H4C 120.0 . .
C3C C4C H4C 120.0 . .
C4C C5C C6C 120.0 . .
C4C C5C H5C 120.0 . .
C6C C5C H5C 120.0 . .
C5C C6C C1C 120.0 . .
C5C C6C C7C 120.0(12) . .
C1C C6C C7C 120.0(12) . .
C6C C7C H7C1 109.5 . .
C6C C7C H7C2 109.5 . .
H7C1 C7C H7C2 109.5 . .
C6C C7C H7C3 109.5 . .
H7C1 C7C H7C3 109.5 . .
H7C2 C7C H7C3 109.5 . .
C2D C1D C6D 120.0 . .
C2D C1D H1D 120.0 . .
C6D C1D H1D 120.0 . .
C3D C2D C1D 120.0 . .
C3D C2D H2D 120.0 . .
C1D C2D H2D 120.0 . .
C4D C3D C2D 120.0 . .
C4D C3D C16 121.3(6) . .
C2D C3D C16 118.6(6) . .
C3D C4D C5D 120.0 . .
C3D C4D H4D 120.0 . .
C5D C4D H4D 120.0 . .
C4D C5D C6D 120.0 . .
C4D C5D H5D 120.0 . .
C6D C5D H5D 120.0 . .
C5D C6D C1D 120.0 . .
C5D C6D C7D 120.6(9) . .
C1D C6D C7D 119.4(9) . .
C6D C7D H7D1 109.5 . .
C6D C7D H7D2 109.5 . .
H7D1 C7D H7D2 109.5 . .
C6D C7D H7D3 109.5 . .
H7D1 C7D H7D3 109.5 . .
H7D2 C7D H7D3 109.5 . .
C2E C1E C3E 104(3) . .
C2E C1E C24 112(3) . .
C3E C1E C24 114(3) . .
C2E C1E H1E 109.0 . .
C3E C1E H1E 109.0 . .
C24 C1E H1E 109.0 . .
C1E C2E H2E1 109.5 . .
C1E C2E H2E2 109.5 . .
H2E1 C2E H2E2 109.5 . .
C1E C2E H2E3 109.5 . .
H2E1 C2E H2E3 109.5 . .
H2E2 C2E H2E3 109.5 . .
C1E C3E H3E1 109.5 . .
C1E C3E H3E2 109.5 . .
H3E1 C3E H3E2 109.5 . .
C1E C3E H3E3 109.5 . .
H3E1 C3E H3E3 109.5 . .
H3E2 C3E H3E3 109.5 . .
C2F C1F C24 115(3) . .
C2F C1F C3F 113(3) . .
C24 C1F C3F 109(3) . .
C2F C1F H1F 106.4 . .
C24 C1F H1F 106.4 . .
C3F C1F H1F 106.4 . .
C1F C2F H2F1 109.5 . .
C1F C2F H2F2 109.5 . .
H2F1 C2F H2F2 109.5 . .
C1F C2F H2F3 109.5 . .
H2F1 C2F H2F3 109.5 . .
H2F2 C2F H2F3 109.5 . .
C1F C3F H3F1 109.5 . .
C1F C3F H3F2 109.5 . .
H3F1 C3F H3F2 109.5 . .
C1F C3F H3F3 109.5 . .
H3F1 C3F H3F3 109.5 . .
H3F2 C3F H3F3 109.5 . .
Cl1M C1M Cl2M 112.0(10) . .
Cl1M C1M Cl3M 107.5(10) . .
Cl2M C1M Cl3M 107.9(10) . .
Cl1M C1M H1M 109.8 . .
Cl2M C1M H1M 109.8 . .
Cl3M C1M H1M 109.8 . .
Cl1R C1R Cl3R 109.8(12) . .
Cl1R C1R Cl2R 109.1(12) . .
Cl3R C1R Cl2R 108.5(12) . .
Cl1R C1R H1R 109.8 . .
Cl3R C1R H1R 109.8 . .
Cl2R C1R H1R 109.8 . .
Cl2N C1N Cl3N 111.7(11) . .
Cl2N C1N Cl1N 109.5(11) . .
Cl3N C1N Cl1N 108.5(11) . .
Cl2N C1N H1N 109.0 . .
Cl3N C1N H1N 109.0 . .
Cl1N C1N H1N 109.0 . .
Cl3P C1P Cl1P 108.6(11) . .
Cl3P C1P Cl2P 108.2(11) . .
Cl1P C1P Cl2P 111.4(12) . .
Cl3P C1P H1P 109.5 . .
Cl1P C1P H1P 109.5 . .
Cl2P C1P H1P 109.5 . .
Cl2Q C1Q Cl1Q 110.7(11) . .
Cl2Q C1Q Cl3Q 109.8(11) . .
Cl1Q C1Q Cl3Q 110.0(11) . .
Cl2Q C1Q H1Q 108.8 . .
Cl1Q C1Q H1Q 108.8 . .
Cl3Q C1Q H1Q 108.8 . .
C29 N21 C23 107.5(9) . .
C29 N21 Rh01 126.4(9) . .
C23 N21 Rh01 125.8(9) . .
C18 N22 C27 108.0(9) . .
C18 N22 Rh01 125.9(8) . .
C27 N22 Rh01 126.0(8) . .
C7 N23 C2 118.1(10) . .
C7 N23 Rh01 120.3(7) . .
C2 N23 Rh01 120.3(7) . .
C9 N00I C17 109.8(9) . .
C9 N00I Rh01 125.4(8) . .
C17 N00I Rh01 124.8(8) . .
C3 N00K C28 107.1(9) . .
C3 N00K Rh01 126.4(8) . .
C28 N00K Rh01 126.6(8) . .
C21 O004 C1 118.3(8) . 4_565
C15 O006 C1 115.2(9) . .
N00K Rh01 N21 90.1(5) . .
N00K Rh01 N22 90.1(4) . .
N21 Rh01 N22 179.5(4) . .
N00K Rh01 N00I 178.8(4) . .
N21 Rh01 N00I 90.2(5) . .
N22 Rh01 N00I 89.6(4) . .
N00K Rh01 N23 93.0(4) . .
N21 Rh01 N23 92.7(4) . .
N22 Rh01 N23 87.8(4) . .
N00I Rh01 N23 85.8(4) . .
N00K Rh01 Cl02 89.2(3) . .
N21 Rh01 Cl02 88.6(3) . .
N22 Rh01 Cl02 90.9(3) . .
N00I Rh01 Cl02 91.9(3) . .
N23 Rh01 Cl02 177.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O004 1.408(14) 3_655
C1 O006 1.434(15) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 N23 1.347(14) .
C2 C8 1.386(16) .
C2 H2 0.9500 .
C3 N00K 1.365(15) .
C3 C31 1.391(17) .
C3 C30 1.443(17) .
C4 C21 1.379(17) .
C4 C26 1.387(17) .
C4 C14 1.550(16) 4_565
C5 C30 1.342(19) .
C5 C28 1.441(18) .
C5 H5 0.9500 .
C6 C33 1.404(18) .
C6 C9 1.429(17) .
C6 H6 0.9500 .
C7 N23 1.337(15) .
C7 C11 1.386(17) .
C7 H7 0.9500 .
C8 C13 1.378(15) .
C8 H8 0.9500 .
C9 N00I 1.359(15) .
C9 C32 1.385(17) .
C10 C19 1.340(17) .
C10 C29 1.449(16) .
C10 H10 0.9500 .
C11 C13 1.383(16) .
C11 H11 0.9500 .
C12 C15 1.381(16) .
C12 C21 1.415(16) .
C12 C13 1.496(16) .
C14 C22 1.517(16) .
C14 C4 1.550(16) 3_655
C14 C24 1.560(17) .
C14 H14 1.0000 .
C15 O006 1.393(14) .
C15 C22 1.405(17) .
C16 C29 1.390(16) .
C16 C28 1.411(17) .
C16 C3D 1.507(12) .
C17 C34 1.354(17) .
C17 N00I 1.376(15) .
C17 C33 1.458(17) .
C18 N22 1.373(16) .
C18 C31 1.385(18) .
C18 C25 1.461(18) .
C19 C23 1.430(17) .
C19 H19 0.9500 .
C20 C25 1.338(18) .
C20 C27 1.418(18) .
C20 H20 0.9500 .
C21 O004 1.372(14) .
C22 C26 1.392(17) .
C23 N21 1.383(17) .
C23 C34 1.408(18) .
C24 C1E 1.53(3) .
C24 C1F 1.58(3) .
C24 H23A 0.9900 .
C24 H23B 0.9900 .
C24 H23C 0.9900 .
C24 H23D 0.9900 .
C25 H25 0.9500 .
C26 H26 0.9500 .
C27 N22 1.376(16) .
C27 C32 1.378(17) .
C28 N00K 1.374(15) .
C29 N21 1.364(17) .
C30 H30 0.9500 .
C31 C3A 1.499(15) .
C32 C3B 1.516(13) .
C33 H33 0.9500 .
C34 C3C 1.530(14) .
C1A C2A 1.3900 .
C1A C6A 1.3900 .
C1A H1A1 0.9500 .
C2A C3A 1.3900 .
C2A H2A 0.9500 .
C3A C4A 1.3900 .
C4A C5A 1.3900 .
C4A H4A 0.9500 .
C5A C6A 1.3900 .
C5A H5A 0.9500 .
C6A C7A 1.52(2) .
C7A H7A1 0.9800 .
C7A H7A2 0.9800 .
C7A H7A3 0.9800 .
C1B C2B 1.3900 .
C1B C6B 1.3900 .
C1B H1B1 0.9500 .
C2B C3B 1.3900 .
C2B H2B 0.9500 .
C3B C4B 1.3900 .
C4B C5B 1.3900 .
C4B H4B 0.9500 .
C5B C6B 1.3900 .
C5B H5B 0.9500 .
C6B C7B 1.517(17) .
C7B H7B1 0.9800 .
C7B H7B2 0.9800 .
C7B H7B3 0.9800 .
C1C C2C 1.3900 .
C1C C6C 1.3900 .
C1C H1C 0.9500 .
C2C C3C 1.3900 .
C2C H2C 0.9500 .
C3C C4C 1.3900 .
C4C C5C 1.3900 .
C4C H4C 0.9500 .
C5C C6C 1.3900 .
C5C H5C 0.9500 .
C6C C7C 1.51(2) .
C7C H7C1 0.9800 .
C7C H7C2 0.9800 .
C7C H7C3 0.9800 .
C1D C2D 1.3900 .
C1D C6D 1.3900 .
C1D H1D 0.9500 .
C2D C3D 1.3900 .
C2D H2D 0.9500 .
C3D C4D 1.3900 .
C4D C5D 1.3900 .
C4D H4D 0.9500 .
C5D C6D 1.3900 .
C5D H5D 0.9500 .
C6D C7D 1.545(14) .
C7D H7D1 0.9800 .
C7D H7D2 0.9800 .
C7D H7D3 0.9800 .
C1E C2E 1.47(5) .
C1E C3E 1.52(5) .
C1E H1E 1.0000 .
C2E H2E1 0.9800 .
C2E H2E2 0.9800 .
C2E H2E3 0.9800 .
C3E H3E1 0.9800 .
C3E H3E2 0.9800 .
C3E H3E3 0.9800 .
C1F C2F 1.54(5) .
C1F C3F 1.64(5) .
C1F H1F 1.0000 .
C2F H2F1 0.9800 .
C2F H2F2 0.9800 .
C2F H2F3 0.9800 .
C3F H3F1 0.9800 .
C3F H3F2 0.9800 .
C3F H3F3 0.9800 .
C1M Cl1M 1.737(12) .
C1M Cl2M 1.739(12) .
C1M Cl3M 1.746(12) .
C1M H1M 1.0000 .
C1R Cl1R 1.733(13) .
C1R Cl3R 1.737(14) .
C1R Cl2R 1.741(13) .
C1R H1R 1.0000 .
C1N Cl2N 1.727(13) .
C1N Cl3N 1.734(13) .
C1N Cl1N 1.738(13) .
C1N H1N 1.0000 .
C1P Cl3P 1.732(14) .
C1P Cl1P 1.734(14) .
C1P Cl2P 1.737(14) .
C1P H1P 1.0000 .
C1Q Cl2Q 1.725(13) .
C1Q Cl1Q 1.729(13) .
C1Q Cl3Q 1.733(13) .
C1Q H1Q 1.0000 .
Cl02 Rh01 2.337(3) .
N21 Rh01 2.028(8) .
N22 Rh01 2.028(8) .
N23 Rh01 2.070(9) .
N00I Rh01 2.034(9) .
N00K Rh01 2.023(9) .
O004 C1 1.408(14) 4_565
