#------------------------------------------------------------------------------
#$Date: 2024-09-20 00:53:48 +0200 (Fri 20 de Sep de 2024) $
#$Revision: 294809 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/70/7717041.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_7717041
loop_
_publ_author_name
'Bru, Francis'
'Charman, Rex S. C.'
'Bourda, Laurens'
'Van Hecke, Kristof'
'Grimaud, Laurence'
'Liptrot, David J.'
'Cazin, Catherine S. J.'
_publ_section_title
;
 A simply accessible organometallic system to gauge electronic properties
 of N-heterocyclic carbenes.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d4dt02584a
_journal_year                    2024
_chemical_formula_moiety         'C34 H47 N2 O3 Rh, C H2 Cl2'
_chemical_formula_sum            'C35 H49 Cl2 N2 O3 Rh'
_chemical_formula_weight         719.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-10-14
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2024-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2980(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.36820(10)
_cell_length_b                   23.62040(10)
_cell_length_c                   14.93630(10)
_cell_measurement_reflns_used    21168
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      73.7610
_cell_measurement_theta_min      3.5690
_cell_volume                     3528.30(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4839
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  31.00   1.00    1.00    --  -41.68  57.00 150.00  101
  2  ω    -87.00  -6.00   1.00    1.00    --  -41.68 125.00-180.00   81
  3  ω     17.00 116.00   1.00    1.00    --   41.68  38.00  60.00   99
  4  ω     33.00 132.00   1.00    2.50    --  106.01 -45.00  60.00   99
  5  ω     30.00 139.00   1.00    2.50    --  106.01 -77.00 -90.00  109
  6  ω    103.00 178.00   1.00    2.50    --  106.01  77.00 -90.00   75
  7  ω     77.00 178.00   1.00    2.50    --  106.01  61.00  60.00  101
  8  ω     30.00 134.00   1.00    2.50    --  106.01 -30.00-120.00  104
  9  ω     14.00 115.00   1.00    1.00    --   41.68  57.00 120.00  101
 10  ω     17.00 116.00   1.00    1.00    --   41.68  38.00 -60.00   99
 11  ω     14.00 115.00   1.00    1.00    --   41.68  57.00-180.00  101
 12  ω     33.00 112.00   1.00    2.50    --  106.01-125.00-120.00   79
 13  ω     77.00 178.00   1.00    2.50    --  106.01  61.00   0.00  101
 14  ω     78.00 178.00   1.00    2.50    --  106.01  30.00 150.00  100
 15  ω     23.00 107.00   1.00    2.50    --  106.01 -94.00  60.00   84
 16  ω     78.00 178.00   1.00    2.50    --  106.01  30.00 -60.00  100
 17  ω     77.00 178.00   1.00    2.50    --  106.01  61.00-150.00  101
 18  ω    -87.00  -6.00   1.00    1.00    --  -41.68 125.00 -60.00   81
 19  ω     14.00 115.00   1.00    1.00    --   41.68  57.00-120.00  101
 20  ω     14.00 115.00   1.00    1.00    --   41.68  57.00 -30.00  101
 21  ω     77.00 149.00   1.00    2.50    --  106.01  61.00-120.00   72
 22  ω     77.00 178.00   1.00    2.50    --  106.01  61.00 -30.00  101
 23  ω     80.00 178.00   1.00    2.50    --  106.01  45.00-180.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0682841000
_diffrn_orient_matrix_UB_12      -0.0582727000
_diffrn_orient_matrix_UB_13      -0.0053402000
_diffrn_orient_matrix_UB_21      -0.0870124000
_diffrn_orient_matrix_UB_22      0.0221096000
_diffrn_orient_matrix_UB_23      0.0616684000
_diffrn_orient_matrix_UB_31      -0.1072436000
_diffrn_orient_matrix_UB_32      0.0191552000
_diffrn_orient_matrix_UB_33      -0.0872284000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            47282
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.823
_diffrn_reflns_theta_min         3.594
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.580
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.310
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       needle
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.73
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         7092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0290
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0375P)²+1.2245P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0689
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6055
_reflns_number_total             7092
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02584a2.cif
_cod_data_source_block           fb226
_cod_database_code               7717041
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CRhNOH
_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_max   0.850
_shelx_estimated_absorpt_t_min   0.106
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C11(H11), C14(H14), C23(H23), C26(H26)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C35(H35A,H35B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C19(H19), C20(H20), C21(H21), C31(H31)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C), C16(H16A,H16B,
 H16C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C33(H33A,H33B,H33C)
;
_olex2_date_sample_data_collection 2022-10-11
_olex2_exptl_crystal_mounting_method 'Mounted on a LythoLoop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.699
_oxdiff_exptl_absorpt_empirical_full_min 0.580
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-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
Rh1 Rh 0.26980(2) 0.33695(2) 0.68804(2) 0.01630(6) Uani 1 1 d . . . . .
O1 O 0.07973(16) 0.36054(7) 0.69073(11) 0.0243(3) Uani 1 1 d . . . . .
O2 O 0.22834(17) 0.36820(6) 0.55321(11) 0.0223(3) Uani 1 1 d . . . . .
O3 O 0.53520(19) 0.29292(8) 0.68395(13) 0.0350(4) Uani 1 1 d . . . . .
N1 N 0.3052(2) 0.35482(7) 0.88452(13) 0.0187(4) Uani 1 1 d . . . . .
N2 N 0.24808(19) 0.26238(7) 0.84144(13) 0.0184(4) Uani 1 1 d . . . . .
C1 C 0.2850(2) 0.31372(9) 0.81895(15) 0.0173(4) Uani 1 1 d . . . . .
C2 C 0.2773(3) 0.34741(10) 0.97598(17) 0.0253(5) Uani 1 1 d . . . . .
H2A H 0.184582 0.359627 0.971972 0.030 Uiso 1 1 calc R U . . .
H2B H 0.338757 0.371549 1.022481 0.030 Uiso 1 1 calc R U . . .
C3 C 0.2947(3) 0.28637(10) 1.00679(17) 0.0266(5) Uani 1 1 d . . . . .
H3A H 0.390263 0.275615 1.020964 0.032 Uiso 1 1 calc R U . . .
H3B H 0.263843 0.281030 1.063542 0.032 Uiso 1 1 calc R U . . .
C4 C 0.2134(3) 0.24992(9) 0.92933(16) 0.0235(5) Uani 1 1 d . . . . .
H4A H 0.231030 0.209486 0.945395 0.028 Uiso 1 1 calc R U . . .
H4B H 0.117030 0.257148 0.921484 0.028 Uiso 1 1 calc R U . . .
C5 C 0.3665(2) 0.40851(9) 0.87230(15) 0.0199(4) Uani 1 1 d . . . . .
C6 C 0.2881(3) 0.45776(9) 0.85772(16) 0.0228(5) Uani 1 1 d . . . . .
C7 C 0.3540(3) 0.50946(10) 0.85744(17) 0.0284(5) Uani 1 1 d . . . . .
H7 H 0.303171 0.543439 0.847728 0.034 Uiso 1 1 calc R U . . .
C8 C 0.4899(3) 0.51247(10) 0.87078(18) 0.0310(6) Uani 1 1 d . . . . .
H8 H 0.532115 0.548165 0.870774 0.037 Uiso 1 1 calc R U . . .
C9 C 0.5655(3) 0.46324(10) 0.88428(18) 0.0278(5) Uani 1 1 d . . . . .
H9 H 0.659463 0.465521 0.892665 0.033 Uiso 1 1 calc R U . . .
C10 C 0.5059(2) 0.41045(9) 0.88573(16) 0.0226(5) Uani 1 1 d . . . . .
C11 C 0.1383(3) 0.45757(10) 0.84517(17) 0.0268(5) Uani 1 1 d . . . . .
H11 H 0.105301 0.417776 0.833340 0.032 Uiso 1 1 calc R U . . .
C12 C 0.0652(3) 0.49437(11) 0.76237(19) 0.0358(6) Uani 1 1 d . . . . .
H12A H 0.093081 0.533910 0.774313 0.054 Uiso 1 1 calc R U . . .
H12B H -0.031519 0.491427 0.753969 0.054 Uiso 1 1 calc R U . . .
H12C H 0.087569 0.481214 0.706060 0.054 Uiso 1 1 calc R U . . .
C13 C 0.1028(3) 0.47925(12) 0.93269(19) 0.0365(6) Uani 1 1 d . . . . .
H13A H 0.146674 0.455487 0.985773 0.055 Uiso 1 1 calc R U . . .
H13B H 0.005700 0.477648 0.923323 0.055 Uiso 1 1 calc R U . . .
H13C H 0.133415 0.518451 0.944792 0.055 Uiso 1 1 calc R U . . .
C14 C 0.5927(3) 0.35770(10) 0.90657(18) 0.0264(5) Uani 1 1 d . . . . .
H14 H 0.536696 0.324907 0.876710 0.032 Uiso 1 1 calc R U . . .
C15 C 0.6367(3) 0.34632(11) 1.0113(2) 0.0347(6) Uani 1 1 d . . . . .
H15A H 0.679831 0.309137 1.022663 0.052 Uiso 1 1 calc R U . . .
H15B H 0.558262 0.346901 1.036283 0.052 Uiso 1 1 calc R U . . .
H15C H 0.699942 0.375634 1.041841 0.052 Uiso 1 1 calc R U . . .
C16 C 0.7149(3) 0.36000(12) 0.8677(2) 0.0393(7) Uani 1 1 d . . . . .
H16A H 0.779334 0.387417 0.903183 0.059 Uiso 1 1 calc R U . . .
H16B H 0.687109 0.371582 0.802390 0.059 Uiso 1 1 calc R U . . .
H16C H 0.756490 0.322488 0.872491 0.059 Uiso 1 1 calc R U . . .
C17 C 0.2492(2) 0.21285(9) 0.78399(16) 0.0196(4) Uani 1 1 d . . . . .
C18 C 0.3660(2) 0.17955(9) 0.80344(16) 0.0215(5) Uani 1 1 d . . . . .
C19 C 0.3620(3) 0.12829(10) 0.75648(17) 0.0264(5) Uani 1 1 d . . . . .
H19 H 0.440497 0.105707 0.767476 0.032 Uiso 1 1 calc R U . . .
C20 C 0.2464(3) 0.10974(10) 0.69438(17) 0.0292(6) Uani 1 1 d . . . . .
H20 H 0.245075 0.074260 0.664191 0.035 Uiso 1 1 calc R U . . .
C21 C 0.1327(3) 0.14281(10) 0.67616(17) 0.0281(5) Uani 1 1 d . . . . .
H21 H 0.053941 0.129943 0.632601 0.034 Uiso 1 1 calc R U . . .
C22 C 0.1310(2) 0.19508(10) 0.72068(16) 0.0232(5) Uani 1 1 d . . . . .
C23 C 0.4922(2) 0.19500(9) 0.87822(18) 0.0245(5) Uani 1 1 d . . . . .
H23 H 0.483713 0.235193 0.896932 0.029 Uiso 1 1 calc R U . . .
C24 C 0.6196(3) 0.19003(12) 0.8450(2) 0.0355(6) Uani 1 1 d . . . . .
H24A H 0.696543 0.202836 0.894363 0.053 Uiso 1 1 calc R U . . .
H24B H 0.610925 0.213609 0.789783 0.053 Uiso 1 1 calc R U . . .
H24C H 0.632787 0.150469 0.829777 0.053 Uiso 1 1 calc R U . . .
C25 C 0.5063(3) 0.15741(11) 0.96438(18) 0.0298(5) Uani 1 1 d . . . . .
H25A H 0.424660 0.159963 0.985435 0.045 Uiso 1 1 calc R U . . .
H25B H 0.582812 0.170282 1.014017 0.045 Uiso 1 1 calc R U . . .
H25C H 0.520578 0.118048 0.948580 0.045 Uiso 1 1 calc R U . . .
C26 C 0.0029(3) 0.22950(11) 0.69876(18) 0.0278(5) Uani 1 1 d . . . . .
H26 H 0.022707 0.266593 0.731819 0.033 Uiso 1 1 calc R U . . .
C27 C -0.1060(3) 0.19953(14) 0.7339(2) 0.0398(7) Uani 1 1 d . . . . .
H27A H -0.187444 0.222616 0.719084 0.060 Uiso 1 1 calc R U . . .
H27B H -0.074695 0.194359 0.801246 0.060 Uiso 1 1 calc R U . . .
H27C H -0.125353 0.162510 0.703693 0.060 Uiso 1 1 calc R U . . .
C28 C -0.0450(3) 0.24157(12) 0.59420(19) 0.0343(6) Uani 1 1 d . . . . .
H28A H -0.063690 0.205730 0.560200 0.051 Uiso 1 1 calc R U . . .
H28B H 0.024813 0.262162 0.574377 0.051 Uiso 1 1 calc R U . . .
H28C H -0.126515 0.264534 0.581290 0.051 Uiso 1 1 calc R U . . .
C29 C -0.1473(3) 0.38605(14) 0.6425(2) 0.0397(7) Uani 1 1 d . . . . .
H29A H -0.184289 0.348347 0.647413 0.060 Uiso 1 1 calc R U . . .
H29B H -0.207644 0.406931 0.591636 0.060 Uiso 1 1 calc R U . . .
H29C H -0.137882 0.406633 0.700837 0.060 Uiso 1 1 calc R U . . .
C30 C -0.0124(3) 0.38030(11) 0.62339(18) 0.0280(5) Uani 1 1 d . . . . .
C31 C 0.0030(3) 0.39607(11) 0.53703(18) 0.0315(6) Uani 1 1 d . . . . .
H31 H -0.073047 0.411669 0.493997 0.038 Uiso 1 1 calc R U . . .
C32 C 0.1200(3) 0.39108(10) 0.50770(17) 0.0260(5) Uani 1 1 d . . . . .
C33 C 0.1222(3) 0.41506(12) 0.41439(18) 0.0354(6) Uani 1 1 d . . . . .
H33A H 0.161288 0.453103 0.422715 0.053 Uiso 1 1 calc R U . . .
H33B H 0.030706 0.417114 0.374381 0.053 Uiso 1 1 calc R U . . .
H33C H 0.176072 0.390533 0.385537 0.053 Uiso 1 1 calc R U . . .
C34 C 0.4319(3) 0.31064(10) 0.68718(16) 0.0233(5) Uani 1 1 d . . . . .
Cl1 Cl 0.30909(7) 0.51966(3) 0.60187(5) 0.03787(15) Uani 1 1 d . . . . .
Cl2 Cl 0.59261(7) 0.49187(3) 0.63852(6) 0.04207(17) Uani 1 1 d . . . . .
C35 C 0.4307(3) 0.46533(10) 0.6280(2) 0.0346(6) Uani 1 1 d . . . . .
H35A H 0.427782 0.446741 0.686815 0.042 Uiso 1 1 calc R U . . .
H35B H 0.409497 0.436442 0.578207 0.042 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 1 -10 0.3177
-2 -1 10 0.3937
6 8 0 0.0220
-6 -8 0 0.0220
-1 15 -1 0.0132
1 -15 1 0.0132
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
O1 Rh1 O2 88.20(6) . . ?
C1 Rh1 O1 83.32(8) . . ?
C1 Rh1 O2 171.18(7) . . ?
C34 Rh1 O1 175.40(9) . . ?
C34 Rh1 O2 94.04(8) . . ?
C34 Rh1 C1 94.59(9) . . ?
C30 O1 Rh1 127.13(16) . . ?
C32 O2 Rh1 126.63(15) . . ?
C1 N1 C2 123.49(19) . . ?
C1 N1 C5 121.63(18) . . ?
C5 N1 C2 114.72(17) . . ?
C1 N2 C4 123.67(18) . . ?
C1 N2 C17 122.23(18) . . ?
C17 N2 C4 113.92(17) . . ?
N1 C1 Rh1 117.90(15) . . ?
N2 C1 Rh1 122.68(16) . . ?
N2 C1 N1 117.83(19) . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 C3 110.94(18) . . ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C2 C3 H3A 110.0 . . ?
C2 C3 H3B 110.0 . . ?
H3A C3 H3B 108.4 . . ?
C4 C3 C2 108.3(2) . . ?
C4 C3 H3A 110.0 . . ?
C4 C3 H3B 110.0 . . ?
N2 C4 C3 110.48(19) . . ?
N2 C4 H4A 109.6 . . ?
N2 C4 H4B 109.6 . . ?
C3 C4 H4A 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
C6 C5 N1 119.3(2) . . ?
C6 C5 C10 121.8(2) . . ?
C10 C5 N1 118.6(2) . . ?
C5 C6 C11 123.4(2) . . ?
C7 C6 C5 117.4(2) . . ?
C7 C6 C11 119.2(2) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.9(2) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 120.1 . . ?
C7 C8 C9 119.8(2) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 121.0(2) . . ?
C10 C9 H9 119.5 . . ?
C5 C10 C14 122.2(2) . . ?
C9 C10 C5 118.1(2) . . ?
C9 C10 C14 119.6(2) . . ?
C6 C11 H11 108.4 . . ?
C6 C11 C12 111.7(2) . . ?
C6 C11 C13 111.2(2) . . ?
C12 C11 H11 108.4 . . ?
C13 C11 H11 108.4 . . ?
C13 C11 C12 108.6(2) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C11 C13 H13A 109.5 . . ?
C11 C13 H13B 109.5 . . ?
C11 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C10 C14 H14 107.5 . . ?
C10 C14 C15 110.7(2) . . ?
C10 C14 C16 113.5(2) . . ?
C15 C14 H14 107.5 . . ?
C16 C14 H14 107.5 . . ?
C16 C14 C15 110.0(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 N2 117.9(2) . . ?
C22 C17 N2 119.9(2) . . ?
C22 C17 C18 121.6(2) . . ?
C17 C18 C23 122.9(2) . . ?
C19 C18 C17 118.1(2) . . ?
C19 C18 C23 118.8(2) . . ?
C18 C19 H19 119.4 . . ?
C20 C19 C18 121.3(2) . . ?
C20 C19 H19 119.4 . . ?
C19 C20 H20 120.1 . . ?
C19 C20 C21 119.9(2) . . ?
C21 C20 H20 120.1 . . ?
C20 C21 H21 119.3 . . ?
C20 C21 C22 121.4(2) . . ?
C22 C21 H21 119.3 . . ?
C17 C22 C21 117.7(2) . . ?
C17 C22 C26 123.0(2) . . ?
C21 C22 C26 119.2(2) . . ?
C18 C23 H23 108.1 . . ?
C18 C23 C24 113.0(2) . . ?
C18 C23 C25 110.41(19) . . ?
C24 C23 H23 108.1 . . ?
C24 C23 C25 109.0(2) . . ?
C25 C23 H23 108.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C22 C26 H26 108.0 . . ?
C22 C26 C27 111.1(2) . . ?
C22 C26 C28 110.4(2) . . ?
C27 C26 H26 108.0 . . ?
C28 C26 H26 108.0 . . ?
C28 C26 C27 111.3(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C30 C29 H29A 109.5 . . ?
C30 C29 H29B 109.5 . . ?
C30 C29 H29C 109.5 . . ?
O1 C30 C29 115.0(2) . . ?
O1 C30 C31 125.6(2) . . ?
C31 C30 C29 119.4(2) . . ?
C30 C31 H31 117.0 . . ?
C30 C31 C32 126.0(2) . . ?
C32 C31 H31 117.0 . . ?
O2 C32 C31 125.9(2) . . ?
O2 C32 C33 115.3(2) . . ?
C31 C32 C33 118.9(2) . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O3 C34 Rh1 177.9(2) . . ?
Cl1 C35 H35A 109.3 . . ?
Cl1 C35 H35B 109.3 . . ?
Cl2 C35 Cl1 111.64(14) . . ?
Cl2 C35 H35A 109.3 . . ?
Cl2 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
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 O1 2.0585(16) . ?
Rh1 O2 2.0806(15) . ?
Rh1 C1 1.997(2) . ?
Rh1 C34 1.796(2) . ?
O1 C30 1.279(3) . ?
O2 C32 1.270(3) . ?
O3 C34 1.162(3) . ?
N1 C1 1.355(3) . ?
N1 C2 1.480(3) . ?
N1 C5 1.451(3) . ?
N2 C1 1.341(3) . ?
N2 C4 1.479(3) . ?
N2 C17 1.453(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C2 C3 1.510(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C3 C4 1.508(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.403(3) . ?
C5 C10 1.406(3) . ?
C6 C7 1.400(3) . ?
C6 C11 1.514(4) . ?
C7 H7 0.9500 . ?
C7 C8 1.372(4) . ?
C8 H8 0.9500 . ?
C8 C9 1.387(4) . ?
C9 H9 0.9500 . ?
C9 C10 1.395(3) . ?
C10 C14 1.521(3) . ?
C11 H11 1.0000 . ?
C11 C12 1.538(3) . ?
C11 C13 1.536(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14 1.0000 . ?
C14 C15 1.533(4) . ?
C14 C16 1.527(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.408(3) . ?
C17 C22 1.400(3) . ?
C18 C19 1.395(3) . ?
C18 C23 1.524(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.379(4) . ?
C20 H20 0.9500 . ?
C20 C21 1.380(4) . ?
C21 H21 0.9500 . ?
C21 C22 1.405(3) . ?
C22 C26 1.518(4) . ?
C23 H23 1.0000 . ?
C23 C24 1.533(3) . ?
C23 C25 1.538(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.538(3) . ?
C26 C28 1.535(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C29 C30 1.506(4) . ?
C30 C31 1.391(4) . ?
C31 H31 0.9500 . ?
C31 C32 1.400(4) . ?
C32 C33 1.510(3) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
Cl1 C35 1.769(3) . ?
Cl2 C35 1.760(3) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
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
Rh1 O1 C30 C29 171.78(18) . . . . ?
Rh1 O1 C30 C31 -8.1(4) . . . . ?
Rh1 O2 C32 C31 -5.0(4) . . . . ?
Rh1 O2 C32 C33 174.31(16) . . . . ?
O1 C30 C31 C32 2.6(5) . . . . ?
N1 C2 C3 C4 -51.9(3) . . . . ?
N1 C5 C6 C7 172.5(2) . . . . ?
N1 C5 C6 C11 -5.8(3) . . . . ?
N1 C5 C10 C9 -172.8(2) . . . . ?
N1 C5 C10 C14 3.9(3) . . . . ?
N2 C17 C18 C19 172.12(19) . . . . ?
N2 C17 C18 C23 -3.2(3) . . . . ?
N2 C17 C22 C21 -171.3(2) . . . . ?
N2 C17 C22 C26 8.5(3) . . . . ?
C1 N1 C2 C3 29.5(3) . . . . ?
C1 N1 C5 C6 109.9(2) . . . . ?
C1 N1 C5 C10 -77.1(3) . . . . ?
C1 N2 C4 C3 -32.6(3) . . . . ?
C1 N2 C17 C18 91.6(3) . . . . ?
C1 N2 C17 C22 -97.2(3) . . . . ?
C2 N1 C1 Rh1 160.41(17) . . . . ?
C2 N1 C1 N2 -5.6(3) . . . . ?
C2 N1 C5 C6 -74.7(3) . . . . ?
C2 N1 C5 C10 98.4(2) . . . . ?
C2 C3 C4 N2 53.2(3) . . . . ?
C4 N2 C1 Rh1 -158.03(17) . . . . ?
C4 N2 C1 N1 7.3(3) . . . . ?
C4 N2 C17 C18 -83.8(2) . . . . ?
C4 N2 C17 C22 87.4(3) . . . . ?
C5 N1 C1 Rh1 -24.5(3) . . . . ?
C5 N1 C1 N2 169.5(2) . . . . ?
C5 N1 C2 C3 -145.9(2) . . . . ?
C5 C6 C7 C8 0.0(4) . . . . ?
C5 C6 C11 C12 -133.3(2) . . . . ?
C5 C6 C11 C13 105.2(3) . . . . ?
C5 C10 C14 C15 -87.8(3) . . . . ?
C5 C10 C14 C16 148.0(2) . . . . ?
C6 C5 C10 C9 0.0(3) . . . . ?
C6 C5 C10 C14 176.8(2) . . . . ?
C6 C7 C8 C9 0.5(4) . . . . ?
C7 C6 C11 C12 48.4(3) . . . . ?
C7 C6 C11 C13 -73.0(3) . . . . ?
C7 C8 C9 C10 -0.8(4) . . . . ?
C8 C9 C10 C5 0.5(4) . . . . ?
C8 C9 C10 C14 -176.3(2) . . . . ?
C9 C10 C14 C15 88.9(3) . . . . ?
C9 C10 C14 C16 -35.3(3) . . . . ?
C10 C5 C6 C7 -0.3(3) . . . . ?
C10 C5 C6 C11 -178.6(2) . . . . ?
C11 C6 C7 C8 178.3(2) . . . . ?
C17 N2 C1 Rh1 27.0(3) . . . . ?
C17 N2 C1 N1 -167.7(2) . . . . ?
C17 N2 C4 C3 142.7(2) . . . . ?
C17 C18 C19 C20 -1.6(3) . . . . ?
C17 C18 C23 C24 -133.4(2) . . . . ?
C17 C18 C23 C25 104.2(2) . . . . ?
C17 C22 C26 C27 -112.7(3) . . . . ?
C17 C22 C26 C28 123.3(2) . . . . ?
C18 C17 C22 C21 -0.5(3) . . . . ?
C18 C17 C22 C26 179.3(2) . . . . ?
C18 C19 C20 C21 1.6(4) . . . . ?
C19 C18 C23 C24 51.3(3) . . . . ?
C19 C18 C23 C25 -71.2(3) . . . . ?
C19 C20 C21 C22 -0.9(4) . . . . ?
C20 C21 C22 C17 0.4(3) . . . . ?
C20 C21 C22 C26 -179.4(2) . . . . ?
C21 C22 C26 C27 67.1(3) . . . . ?
C21 C22 C26 C28 -56.9(3) . . . . ?
C22 C17 C18 C19 1.1(3) . . . . ?
C22 C17 C18 C23 -174.3(2) . . . . ?
C23 C18 C19 C20 173.9(2) . . . . ?
C29 C30 C31 C32 -177.2(3) . . . . ?
C30 C31 C32 O2 4.6(5) . . . . ?
C30 C31 C32 C33 -174.7(3) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
2.2791 1.3526 -9.6259 -0.1830 -0.7620 0.6211
-2.1318 -1.4655 9.6345 0.1795 0.7472 -0.6398
5.6877 7.6006 -0.2923 -0.8297 -0.3449 -0.4389
-5.6877 -7.6006 0.2923 0.8297 0.3449 0.4389
-1.2125 14.8900 -1.0195 -0.7794 0.3718 0.5042
1.2125 -14.8900 1.0195 0.7794 -0.3718 -0.5042
