#------------------------------------------------------------------------------
#$Date: 2020-09-17 02:11:54 +0300 (Thu, 17 Sep 2020) $
#$Revision: 256465 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/03/87/4038758.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_4038758
loop_
_publ_author_name
'Wertz, Benjamin'
'Ren, Zhi'
'Bacsa, John'
'Musaev, Djamaladdin G.'
'Davies, Huw M. L.'
_publ_section_title
;
 Comparison of 1,2-Diarylcyclopropanecarboxylates with
 1,2,2-Triarylcyclopropanecarboxylates as Chiral Ligands for
 Dirhodium-Catalyzed Cyclopropanation and C-H Functionalization.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01276
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C64 H52 O8 Rh2, 2(C7 H8)'
_chemical_formula_sum            'C78 H68 O8 Rh2'
_chemical_formula_weight         1339.14
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-09-01
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   31.5424(7)
_cell_length_b                   8.3838(2)
_cell_length_c                   11.9960(3)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.43
_cell_measurement_theta_min      3.68
_cell_volume                     3172.28(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2014.11 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'd8 VENTURE'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            21186
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.500
_diffrn_reflns_theta_min         2.802
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           35
_diffrn_source_voltage           45
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.671
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       prism
_exptl_crystal_F_000             1380
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.860
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 2256 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(8)
_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     445
_refine_ls_number_reflns         6408
_refine_ls_number_restraints     296
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+3.5901P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0802
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.740
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.970
_reflns_number_gt                5736
_reflns_number_total             6408
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            jo0c01276_si_002.cif
_cod_data_source_block           bdw-unknown
_cod_database_code               4038758
_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.
;
_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. Restrained distances
 C8S-C9S
 1.506 with sigma of 0.02
 C8S-C14S
 2.525 with sigma of 0.04
 C8S-C10S
 2.524 with sigma of 0.04
 C9S-C14S
 1.392 with sigma of 0.02
 C9S-C13S
 2.418 with sigma of 0.04
 C9S-C10S
 1.395 with sigma of 0.02
 C9S-C11S
 2.412 with sigma of 0.04
 C14S-C13S
 1.378 with sigma of 0.02
 C14S-C12S
 2.391 with sigma of 0.04
 C13S-C12S
 1.39 with sigma of 0.02
 C13S-C11S
 2.396 with sigma of 0.04
 C12S-C11S
 1.381 with sigma of 0.02
 C12S-C10S
 2.397 with sigma of 0.04
 C11S-C10S
 1.38 with sigma of 0.02
 C1S'-C2S'
 1.51 with sigma of 0.02
 C2S'-C7S' \\sim C7S'-C6S' \\sim C6S'-C5S' \\sim C5S'-C4S' \\sim C4S'-C3S'
\\sim C3S'-C2S'
 with sigma of 0.02
 C2S'-C4S' \\sim C2S'-C6S' \\sim C3S'-C5S' \\sim C7S'-C3S' \\sim C6S'-C4S'
\\sim C7S'-C5S'
 with sigma of 0.04
 C1S'-C3S' \\sim C1S'-C7S'
 with sigma of 0.04
3. Restrained planarity
 C1S', C2S', C7S', C6S', C5S', C4S', C3S'
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1S' \\sim C2S' \\sim C7S' \\sim C6S' \\sim C5S' \\sim C4S' \\sim C3S': within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C31) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C9S) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C6S') \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C5S') \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C6S') = Uanis(C4S')
Uanis(C1S) = Uanis(C2S) = Uanis(C7S) = Uanis(C6S) = Uanis(C5S) = Uanis(C4S) =
Uanis(C3S)
Uanis(C7S') = Uanis(C7S)
Uanis(C2S) = Uanis(C2S')
Uanis(C3S) = Uanis(C3S')
Uanis(C1S) = Uanis(C1S')
5. Rigid body (RIGU) restrains
 C1S', C2S', C7S', C6S', C5S', C4S', C3S'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C18, C28, C29, C30, C31, C32
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C9S, C8S, C14S, C10S, C13S, C11S, C12S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C2S, C1S', C2S', C7S', C3S', C6S', C4S', C7S, C4S, C3S, C5S', C1S, C6S, C5S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Fixed Sof: C9S(0.5) C11S(0.5) H11S(0.5) C13S(0.5) H13S(0.5) C8S(0.5)
 H8SA(0.5) H8SB(0.5) H8SC(0.5) C14S(0.5) H14S(0.5) C12S(0.5) H12S(0.5)
 C10S(0.5) H10S(0.5) C1S'(0.25) H1SA(0.25) H1SB(0.25) H1SC(0.25) C2S'(0.25)
 C7S'(0.25) H7S'(0.25) C6S'(0.25) H6S'(0.25) C5S'(0.25) H5S'(0.25) C4S'(0.25)
 H4S'(0.25) C3S'(0.25) H3S'(0.25) C1S(0.25) H1SD(0.25) H1SE(0.25) H1SF(0.25)
 C2S(0.25) C7S(0.25) H7S(0.25) C6S(0.25) H6S(0.25) C5S(0.25) H5S(0.25)
 C4S(0.25) H4S(0.25) C3S(0.25) H3S(0.25)
7.a Free rotating group:
 C1S(C2S,C7S,C6S,C5S,C4S,C3S)
7.b Ternary CH refined with riding coordinates:
 C3(H3), C19(H19)
7.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C20(H20A,H20B)
7.d Aromatic/amide H refined with riding coordinates:
 C25(H25), C29(H29), C11S(H11S), C7(H7), C31(H31), C8(H8), C9(H9), C6(H6),
 C13S(H13S), C24(H24), C12(H12), C26(H26), C13(H13), C28(H28), C14(H14),
 C30(H30), C15(H15), C32(H32), C16(H16), C10(H10), C14S(H14S), C12S(H12S),
 C22(H22), C10S(H10S), C23(H23), C7S'(H7S'), C6S'(H6S'), C5S'(H5S'), C4S'(H4S'),
  C3S'(H3S'), C7S(H7S), C6S(H6S), C5S(H5S), C4S(H4S), C3S(H3S)
7.e Idealised Me refined as rotating group:
 C8S(H8SA,H8SB,H8SC), C1S'(H1SA,H1SB,H1SC), C1S(H1SD,H1SE,H1SF)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id BDW-unknown
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
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 0.56022(17) 0.5429(7) 0.5329(5) 0.0255(13) Uani 1 1 d . . . . .
C25 C 0.2611(3) 0.4989(16) 0.0419(7) 0.069(3) Uani 1 1 d . . . . .
H25 H 0.2471 0.5168 -0.0272 0.083 Uiso 1 1 calc R . . . .
C2 C 0.59750(16) 0.5622(7) 0.6109(7) 0.0273(12) Uani 1 1 d . . . . .
O1 O 0.54112(12) 0.6666(5) 0.5020(4) 0.0274(10) Uani 1 1 d . . . . .
C29 C 0.3619(3) 0.0264(11) 0.1974(9) 0.065(2) Uani 1 1 d . U . . .
H29 H 0.3556 -0.0463 0.2558 0.078 Uiso 1 1 calc R . . . .
C9S C 0.4982(7) 0.3653(17) -0.1140(13) 0.050(3) Uani 0.5 1 d D U P A -1
C3 C 0.62635(18) 0.7098(8) 0.5852(6) 0.0331(16) Uani 1 1 d . . . . .
H3 H 0.6164 0.7770 0.5215 0.040 Uiso 1 1 calc R . . . .
C5 C 0.67331(17) 0.7036(7) 0.5983(6) 0.0342(14) Uani 1 1 d . . . . .
C11S C 0.5021(7) 0.6159(18) -0.0179(13) 0.057(4) Uani 0.5 1 d D U P A -1
H11S H 0.5044 0.6744 0.0496 0.069 Uiso 0.5 1 calc R . P A -1
C4 C 0.59687(18) 0.7083(8) 0.6841(6) 0.0326(14) Uani 1 1 d . . . . .
H4A H 0.6098 0.6992 0.7590 0.039 Uiso 1 1 calc R . . . .
H4B H 0.5714 0.7773 0.6806 0.039 Uiso 1 1 calc R . . . .
C27 C 0.38916(18) 0.2817(8) 0.1364(6) 0.0347(14) Uani 1 1 d . U . . .
C7 C 0.7377(2) 0.6424(13) 0.7005(7) 0.057(2) Uani 1 1 d . . . . .
H7 H 0.7512 0.5968 0.7638 0.068 Uiso 1 1 calc R . . . .
C31 C 0.3618(4) 0.0895(15) 0.0078(12) 0.094(3) Uani 1 1 d . U . . .
H31 H 0.3546 0.0626 -0.0668 0.113 Uiso 1 1 calc R . . . .
C8 C 0.76162(19) 0.7101(10) 0.6167(9) 0.0525(19) Uani 1 1 d . . . . .
H8 H 0.7917 0.7118 0.6228 0.063 Uiso 1 1 calc R . . . .
O3 O 0.44794(13) 0.6051(5) 0.2736(4) 0.0299(11) Uani 1 1 d . . . . .
C9 C 0.7423(2) 0.7753(10) 0.5243(7) 0.0477(19) Uani 1 1 d . . . . .
H9 H 0.7588 0.8236 0.4673 0.057 Uiso 1 1 calc R . . . .
C6 C 0.69378(18) 0.6412(11) 0.6918(6) 0.0450(16) Uani 1 1 d . . . . .
H6 H 0.6774 0.5971 0.7507 0.054 Uiso 1 1 calc R . . . .
Rh1 Rh 0.49379(2) 0.64061(5) 0.38874(4) 0.02330(10) Uani 1 1 d . . . . .
C13S C 0.4987(6) 0.6090(19) -0.2130(13) 0.044(3) Uani 0.5 1 d D U P A -1
H13S H 0.4973 0.6659 -0.2814 0.053 Uiso 0.5 1 calc R . P A -1
C11 C 0.61584(17) 0.4078(8) 0.6499(6) 0.0294(14) Uani 1 1 d . . . . .
C24 C 0.2402(2) 0.4248(11) 0.1270(8) 0.063(2) Uani 1 1 d . . . . .
H24 H 0.2120 0.3879 0.1162 0.076 Uiso 1 1 calc R . . . .
C12 C 0.64054(18) 0.3173(8) 0.5795(6) 0.0343(16) Uani 1 1 d . . . . .
H12 H 0.6480 0.3577 0.5082 0.041 Uiso 1 1 calc R . . . .
C26 C 0.3030(2) 0.5482(11) 0.0563(7) 0.053(2) Uani 1 1 d . . . . .
H26 H 0.3178 0.5977 -0.0034 0.064 Uiso 1 1 calc R . . . .
C13 C 0.65468(17) 0.1664(8) 0.6122(7) 0.0409(15) Uani 1 1 d . . . . .
H13 H 0.6715 0.1040 0.5631 0.049 Uiso 1 1 calc R . . . .
C28 C 0.3798(2) 0.1747(9) 0.2215(7) 0.0458(16) Uani 1 1 d . U . . .
H28 H 0.3857 0.2027 0.2967 0.055 Uiso 1 1 calc R . . . .
C14 C 0.6441(2) 0.1092(9) 0.7153(7) 0.0468(19) Uani 1 1 d . . . . .
H14 H 0.6537 0.0066 0.7376 0.056 Uiso 1 1 calc R . . . .
C30 C 0.3533(3) -0.0138(12) 0.0885(9) 0.076(2) Uani 1 1 d . U . . .
H30 H 0.3413 -0.1149 0.0713 0.092 Uiso 1 1 calc R . . . .
C15 C 0.6197(2) 0.1988(11) 0.7871(7) 0.052(2) Uani 1 1 d . . . . .
H15 H 0.6124 0.1581 0.8584 0.062 Uiso 1 1 calc R . . . .
C32 C 0.3806(4) 0.2341(13) 0.0286(9) 0.076(3) Uani 1 1 d . U . . .
H32 H 0.3878 0.3021 -0.0319 0.091 Uiso 1 1 calc R . . . .
C16 C 0.60587(19) 0.3501(10) 0.7543(5) 0.0390(14) Uani 1 1 d . . . . .
H16 H 0.5895 0.4133 0.8041 0.047 Uiso 1 1 calc R . . . .
O2 O 0.55126(12) 0.4000(5) 0.5070(4) 0.0284(11) Uani 1 1 d . . . . .
C17 C 0.43988(18) 0.4643(8) 0.2421(5) 0.0279(14) Uani 1 1 d . . . . .
O4 O 0.46053(12) 0.3402(6) 0.2689(4) 0.0277(10) Uani 1 1 d . . . . .
C18 C 0.40349(19) 0.4460(8) 0.1624(6) 0.0298(13) Uani 1 1 d . U . . .
C10 C 0.69814(19) 0.7692(9) 0.5157(7) 0.0402(17) Uani 1 1 d . . . . .
H10 H 0.6849 0.8116 0.4510 0.048 Uiso 1 1 calc R . . . .
C19 C 0.3684(2) 0.5740(8) 0.1749(6) 0.0347(15) Uani 1 1 d . . . . .
H19 H 0.3731 0.6539 0.2355 0.042 Uiso 1 1 calc R . . . .
C8S C 0.4969(6) 0.1820(17) -0.1108(16) 0.070(4) Uani 0.5 1 d D U P A -1
H8SA H 0.4903 0.1410 -0.1854 0.105 Uiso 0.5 1 calc GR . P A -1
H8SB H 0.4749 0.1472 -0.0584 0.105 Uiso 0.5 1 calc GR . P A -1
H8SC H 0.5245 0.1408 -0.0867 0.105 Uiso 0.5 1 calc GR . P A -1
C20 C 0.3984(2) 0.5823(9) 0.0813(6) 0.0431(19) Uani 1 1 d . . . . .
H20A H 0.4200 0.6679 0.0830 0.052 Uiso 1 1 calc R . . . .
H20B H 0.3874 0.5568 0.0060 0.052 Uiso 1 1 calc R . . . .
C14S C 0.4976(8) 0.4465(17) -0.2166(12) 0.046(3) Uani 0.5 1 d D U P A -1
H14S H 0.4965 0.3905 -0.2854 0.055 Uiso 0.5 1 calc R . P A -1
C21 C 0.3231(2) 0.5249(8) 0.1574(6) 0.0348(15) Uani 1 1 d . . . . .
C12S C 0.5015(5) 0.693(2) -0.1176(14) 0.047(3) Uani 0.5 1 d D U P A -1
H12S H 0.5031 0.8063 -0.1200 0.057 Uiso 0.5 1 calc R . P A -1
C22 C 0.3008(2) 0.4557(10) 0.2427(7) 0.0464(19) Uani 1 1 d . . . . .
H22 H 0.3139 0.4431 0.3135 0.056 Uiso 1 1 calc R . . . .
C10S C 0.4994(6) 0.4518(15) -0.0158(11) 0.047(3) Uani 0.5 1 d D U P A -1
H10S H 0.4983 0.3976 0.0537 0.057 Uiso 0.5 1 calc R . P A -1
C23 C 0.2595(2) 0.4037(12) 0.2271(8) 0.061(3) Uani 1 1 d . . . . .
H23 H 0.2447 0.3534 0.2864 0.073 Uiso 1 1 calc R . . . .
C1S' C 0.5076(9) 0.011(4) 0.2042(15) 0.0283(17) Uani 0.25 1 d D U P B -1
H1SA H 0.4921 -0.0802 0.1732 0.042 Uiso 0.25 1 calc GR . P B -1
H1SB H 0.5372 0.0063 0.1799 0.042 Uiso 0.25 1 calc GR . P B -1
H1SC H 0.4947 0.1103 0.1780 0.042 Uiso 0.25 1 calc GR . P B -1
C2S' C 0.5057(8) 0.005(3) 0.3295(15) 0.0283(17) Uani 0.25 1 d D U P B -1
C7S' C 0.4711(9) -0.061(5) 0.385(2) 0.0283(17) Uani 0.25 1 d D U P B -1
H7S' H 0.4485 -0.1048 0.3421 0.034 Uiso 0.25 1 calc R . P B -1
C6S' C 0.4688(15) -0.066(6) 0.500(3) 0.033(3) Uani 0.25 1 d D U P B -1
H6S' H 0.4445 -0.1104 0.5352 0.040 Uiso 0.25 1 calc R . P B -1
C5S' C 0.5017(18) -0.006(8) 0.5647(15) 0.034(3) Uani 0.25 1 d D U P B -1
H5S' H 0.5000 -0.0071 0.6437 0.041 Uiso 0.25 1 calc R . P B -1
C4S' C 0.5370(14) 0.057(7) 0.511(2) 0.033(3) Uani 0.25 1 d D U P B -1
H4S' H 0.5606 0.0920 0.5539 0.040 Uiso 0.25 1 calc R . P B -1
C3S' C 0.5381(9) 0.067(5) 0.395(2) 0.0283(17) Uani 0.25 1 d D U P B -1
H3S' H 0.5614 0.1183 0.3605 0.034 Uiso 0.25 1 calc R . P B -1
C1S C 0.5202(8) 0.041(3) 0.2045(13) 0.0283(17) Uani 0.25 1 d . U P C -2
H1SD H 0.5421 0.1230 0.1955 0.042 Uiso 0.25 1 calc GR . P C -2
H1SE H 0.4946 0.0731 0.1641 0.042 Uiso 0.25 1 calc GR . P C -2
H1SF H 0.5306 -0.0605 0.1746 0.042 Uiso 0.25 1 calc GR . P C -2
C2S C 0.5100(5) 0.0217(19) 0.3264(13) 0.0283(17) Uani 0.25 1 d G U P C -2
C7S C 0.5384(6) 0.070(3) 0.4085(14) 0.0283(17) Uani 0.25 1 d G U P C -2
H7S H 0.5647 0.1161 0.3869 0.034 Uiso 0.25 1 calc R . P C -2
C6S C 0.5295(6) 0.052(4) 0.5202(14) 0.0283(17) Uani 0.25 1 d G U P C -2
H6S H 0.5494 0.0857 0.5748 0.034 Uiso 0.25 1 calc R . P C -2
C5S C 0.4912(5) -0.016(3) 0.5525(13) 0.0283(17) Uani 0.25 1 d G U P C -2
H5S H 0.4849 -0.0293 0.6293 0.034 Uiso 0.25 1 calc R . P C -2
C4S C 0.4625(5) -0.064(3) 0.4723(15) 0.0283(17) Uani 0.25 1 d G U P C -2
H4S H 0.4363 -0.1101 0.4942 0.034 Uiso 0.25 1 calc R . P C -2
C3S C 0.4717(5) -0.046(3) 0.3606(15) 0.0283(17) Uani 0.25 1 d G U P C -2
H3S H 0.4518 -0.0802 0.3062 0.034 Uiso 0.25 1 calc R . P C -2
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'
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_
_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 C1 C2 117.9(5) . . ?
O1 C1 O2 126.9(6) . . ?
O2 C1 C2 115.2(5) . . ?
C24 C25 H25 120.0 . . ?
C24 C25 C26 120.0(8) . . ?
C26 C25 H25 120.0 . . ?
C1 C2 C3 114.5(6) . . ?
C4 C2 C1 115.9(5) . . ?
C4 C2 C3 58.7(4) . . ?
C11 C2 C1 113.8(5) . . ?
C11 C2 C3 121.4(5) . . ?
C11 C2 C4 121.8(6) . . ?
C1 O1 Rh1 117.5(4) . . ?
C28 C29 H29 120.2 . . ?
C30 C29 H29 120.2 . . ?
C30 C29 C28 119.6(10) . . ?
C14S C9S C8S 120.3(14) . . ?
C10S C9S C8S 120.3(14) . . ?
C10S C9S C14S 119.4(12) . . ?
C2 C3 H3 114.4 . . ?
C5 C3 C2 121.9(6) . . ?
C5 C3 H3 114.4 . . ?
C5 C3 C4 122.0(6) . . ?
C4 C3 C2 58.7(4) . . ?
C4 C3 H3 114.4 . . ?
C6 C5 C3 123.9(6) . . ?
C10 C5 C3 118.4(7) . . ?
C10 C5 C6 117.7(6) . . ?
C12S C11S H11S 120.3 . . ?
C12S C11S C10S 119.4(16) . . ?
C10S C11S H11S 120.3 . . ?
C2 C4 C3 62.7(4) . . ?
C2 C4 H4A 117.5 . . ?
C2 C4 H4B 117.5 . . ?
C3 C4 H4A 117.5 . . ?
C3 C4 H4B 117.5 . . ?
H4A C4 H4B 114.6 . . ?
C28 C27 C18 120.6(7) . . ?
C32 C27 C28 117.4(8) . . ?
C32 C27 C18 121.7(8) . . ?
C8 C7 H7 120.2 . . ?
C8 C7 C6 119.6(8) . . ?
C6 C7 H7 120.2 . . ?
C30 C31 H31 118.9 . . ?
C30 C31 C32 122.1(12) . . ?
C32 C31 H31 118.9 . . ?
C7 C8 H8 119.7 . . ?
C9 C8 C7 120.6(6) . . ?
C9 C8 H8 119.7 . . ?
C17 O3 Rh1 119.0(4) . . ?
C8 C9 H9 120.5 . . ?
C8 C9 C10 119.1(8) . . ?
C10 C9 H9 120.5 . . ?
C5 C6 H6 119.4 . . ?
C7 C6 C5 121.2(7) . . ?
C7 C6 H6 119.4 . . ?
O1 Rh1 Rh1 89.16(13) . 2_665 ?
O1 Rh1 O2 93.73(18) . 2_665 ?
O1 Rh1 O4 86.78(15) . 2_665 ?
O3 Rh1 O1 177.33(19) . . ?
O3 Rh1 Rh1 88.41(13) . 2_665 ?
O3 Rh1 O2 87.26(15) . 2_665 ?
O3 Rh1 O4 92.02(17) . 2_665 ?
O2 Rh1 Rh1 87.09(12) 2_665 2_665 ?
O2 Rh1 O4 174.9(2) 2_665 2_665 ?
O4 Rh1 Rh1 87.82(15) 2_665 2_665 ?
C14S C13S H13S 118.2 . . ?
C12S C13S H13S 118.2 . . ?
C12S C13S C14S 123.5(16) . . ?
C12 C11 C2 120.3(6) . . ?
C12 C11 C16 119.5(6) . . ?
C16 C11 C2 120.1(6) . . ?
C25 C24 H24 119.9 . . ?
C23 C24 C25 120.3(7) . . ?
C23 C24 H24 119.9 . . ?
C11 C12 H12 119.7 . . ?
C11 C12 C13 120.5(7) . . ?
C13 C12 H12 119.7 . . ?
C25 C26 H26 120.0 . . ?
C21 C26 C25 120.1(8) . . ?
C21 C26 H26 120.0 . . ?
C12 C13 H13 120.2 . . ?
C14 C13 C12 119.6(7) . . ?
C14 C13 H13 120.2 . . ?
C29 C28 H28 119.7 . . ?
C27 C28 C29 120.5(8) . . ?
C27 C28 H28 119.7 . . ?
C13 C14 H14 119.7 . . ?
C13 C14 C15 120.6(7) . . ?
C15 C14 H14 119.7 . . ?
C29 C30 H30 120.2 . . ?
C31 C30 C29 119.6(10) . . ?
C31 C30 H30 120.2 . . ?
C14 C15 H15 120.2 . . ?
C14 C15 C16 119.6(8) . . ?
C16 C15 H15 120.2 . . ?
C27 C32 H32 119.7 . . ?
C31 C32 C27 120.7(12) . . ?
C31 C32 H32 119.7 . . ?
C11 C16 C15 120.2(7) . . ?
C11 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C1 O2 Rh1 119.0(4) . 2_665 ?
O3 C17 O4 125.9(6) . . ?
O3 C17 C18 116.0(6) . . ?
O4 C17 C18 118.0(6) . . ?
C17 O4 Rh1 118.4(4) . 2_665 ?
C27 C18 C17 117.5(5) . . ?
C27 C18 C19 116.5(5) . . ?
C27 C18 C20 122.4(6) . . ?
C17 C18 C19 114.4(6) . . ?
C17 C18 C20 114.5(6) . . ?
C20 C18 C19 57.4(5) . . ?
C5 C10 C9 121.8(7) . . ?
C5 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
C18 C19 H19 115.3 . . ?
C20 C19 C18 59.9(5) . . ?
C20 C19 H19 115.3 . . ?
C20 C19 C21 121.2(6) . . ?
C21 C19 C18 118.5(6) . . ?
C21 C19 H19 115.3 . . ?
C9S C8S H8SA 109.5 . . ?
C9S C8S H8SB 109.5 . . ?
C9S C8S H8SC 109.5 . . ?
H8SA C8S H8SB 109.5 . . ?
H8SA C8S H8SC 109.5 . . ?
H8SB C8S H8SC 109.5 . . ?
C18 C20 H20A 117.5 . . ?
C18 C20 H20B 117.5 . . ?
C19 C20 C18 62.7(4) . . ?
C19 C20 H20A 117.5 . . ?
C19 C20 H20B 117.5 . . ?
H20A C20 H20B 114.6 . . ?
C9S C14S H14S 121.5 . . ?
C13S C14S C9S 117.1(16) . . ?
C13S C14S H14S 121.5 . . ?
C26 C21 C19 121.4(7) . . ?
C22 C21 C26 118.7(6) . . ?
C22 C21 C19 119.9(6) . . ?
C11S C12S H12S 120.1 . . ?
C13S C12S C11S 119.8(14) . . ?
C13S C12S H12S 120.1 . . ?
C21 C22 H22 119.6 . . ?
C21 C22 C23 120.9(7) . . ?
C23 C22 H22 119.6 . . ?
C9S C10S H10S 119.7 . . ?
C11S C10S C9S 120.6(15) . . ?
C11S C10S H10S 119.7 . . ?
C24 C23 C22 120.0(8) . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
H1SA C1S' H1SB 109.5 . . ?
H1SA C1S' H1SC 109.5 . . ?
H1SB C1S' H1SC 109.5 . . ?
C2S' C1S' H1SA 109.5 . . ?
C2S' C1S' H1SB 109.5 . . ?
C2S' C1S' H1SC 109.5 . . ?
C7S' C2S' C1S' 121.3(19) . . ?
C7S' C2S' C3S' 117.0(13) . . ?
C3S' C2S' C1S' 121.7(19) . . ?
C2S' C7S' H7S' 119.1 . . ?
C6S' C7S' C2S' 121.8(18) . . ?
C6S' C7S' H7S' 119.1 . . ?
C7S' C6S' H6S' 119.8 . . ?
C7S' C6S' C5S' 120.4(18) . . ?
C5S' C6S' H6S' 119.8 . . ?
C6S' C5S' H5S' 120.7 . . ?
C4S' C5S' C6S' 118.6(14) . . ?
C4S' C5S' H5S' 120.7 . . ?
C5S' C4S' H4S' 119.9 . . ?
C5S' C4S' C3S' 120.2(18) . . ?
C3S' C4S' H4S' 119.9 . . ?
C2S' C3S' C4S' 121.7(18) . . ?
C2S' C3S' H3S' 119.2 . . ?
C4S' C3S' H3S' 119.2 . . ?
H1SD C1S H1SE 109.5 . . ?
H1SD C1S H1SF 109.5 . . ?
H1SE C1S H1SF 109.5 . . ?
C2S C1S H1SD 109.5 . . ?
C2S C1S H1SE 109.5 . . ?
C2S C1S H1SF 109.5 . . ?
C7S C2S C1S 121.1 . . ?
C7S C2S C3S 117.9 . . ?
C3S C2S C1S 120.9 . . ?
C2S C7S H7S 119.2 . . ?
C6S C7S C2S 121.6 . . ?
C6S C7S H7S 119.2 . . ?
C7S C6S H6S 120.2 . . ?
C7S C6S C5S 119.6 . . ?
C5S C6S H6S 120.2 . . ?
C6S C5S H5S 120.2 . . ?
C4S C5S C6S 119.7 . . ?
C4S C5S H5S 120.2 . . ?
C5S C4S H4S 119.8 . . ?
C3S C4S C5S 120.4 . . ?
C3S C4S H4S 119.8 . . ?
C2S C3S H3S 119.6 . . ?
C4S C3S C2S 120.8 . . ?
C4S C3S H3S 119.6 . . ?
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
C1 C2 1.511(9) . ?
C1 O1 1.255(7) . ?
C1 O2 1.270(7) . ?
C25 H25 0.9500 . ?
C25 C24 1.365(13) . ?
C25 C26 1.397(11) . ?
C2 C3 1.567(8) . ?
C2 C4 1.507(9) . ?
C2 C11 1.493(8) . ?
O1 Rh1 2.030(4) . ?
C29 H29 0.9500 . ?
C29 C28 1.397(11) . ?
C29 C30 1.375(14) . ?
C9S C8S 1.538(17) . ?
C9S C14S 1.407(17) . ?
C9S C10S 1.383(17) . ?
C3 H3 1.0000 . ?
C3 C5 1.490(8) . ?
C3 C4 1.507(10) . ?
C5 C6 1.396(10) . ?
C5 C10 1.378(10) . ?
C11S H11S 0.9500 . ?
C11S C12S 1.361(18) . ?
C11S C10S 1.378(18) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C27 C28 1.391(11) . ?
C27 C32 1.380(12) . ?
C27 C18 1.483(9) . ?
C7 H7 0.9500 . ?
C7 C8 1.378(12) . ?
C7 C6 1.391(9) . ?
C31 H31 0.9500 . ?
C31 C30 1.327(16) . ?
C31 C32 1.373(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.378(13) . ?
O3 Rh1 2.022(4) . ?
O3 C17 1.266(8) . ?
C9 H9 0.9500 . ?
C9 C10 1.398(9) . ?
C6 H6 0.9500 . ?
Rh1 Rh1 2.3901(8) 2_665 ?
Rh1 O2 2.036(4) 2_665 ?
Rh1 O4 2.042(4) 2_665 ?
C13S H13S 0.9500 . ?
C13S C14S 1.364(17) . ?
C13S C12S 1.347(18) . ?
C11 C12 1.377(9) . ?
C11 C16 1.379(10) . ?
C24 H24 0.9500 . ?
C24 C23 1.357(13) . ?
C12 H12 0.9500 . ?
C12 C13 1.397(9) . ?
C26 H26 0.9500 . ?
C26 C21 1.381(10) . ?
C13 H13 0.9500 . ?
C13 C14 1.368(11) . ?
C28 H28 0.9500 . ?
C14 H14 0.9500 . ?
C14 C15 1.378(11) . ?
C30 H30 0.9500 . ?
C15 H15 0.9500 . ?
C15 C16 1.398(11) . ?
C32 H32 0.9500 . ?
C16 H16 0.9500 . ?
O2 Rh1 2.036(4) 2_665 ?
C17 O4 1.269(8) . ?
C17 C18 1.502(9) . ?
O4 Rh1 2.042(4) 2_665 ?
C18 C19 1.550(9) . ?
C18 C20 1.509(9) . ?
C10 H10 0.9500 . ?
C19 H19 1.0000 . ?
C19 C20 1.470(10) . ?
C19 C21 1.501(9) . ?
C8S H8SA 0.9800 . ?
C8S H8SB 0.9800 . ?
C8S H8SC 0.9800 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C14S H14S 0.9500 . ?
C21 C22 1.371(10) . ?
C12S H12S 0.9500 . ?
C22 H22 0.9500 . ?
C22 C23 1.388(10) . ?
C10S H10S 0.9500 . ?
C23 H23 0.9500 . ?
C1S' H1SA 0.9800 . ?
C1S' H1SB 0.9800 . ?
C1S' H1SC 0.9800 . ?
C1S' C2S' 1.505(19) . ?
C2S' C7S' 1.391(17) . ?
C2S' C3S' 1.393(17) . ?
C7S' H7S' 0.9500 . ?
C7S' C6S' 1.387(18) . ?
C6S' H6S' 0.9500 . ?
C6S' C5S' 1.391(18) . ?
C5S' H5S' 0.9500 . ?
C5S' C4S' 1.387(18) . ?
C4S' H4S' 0.9500 . ?
C4S' C3S' 1.393(18) . ?
C3S' H3S' 0.9500 . ?
C1S H1SD 0.9800 . ?
C1S H1SE 0.9800 . ?
C1S H1SF 0.9800 . ?
C1S C2S 1.5061 . ?
C2S C7S 1.3920 . ?
C2S C3S 1.3950 . ?
C7S H7S 0.9500 . ?
C7S C6S 1.3774 . ?
C6S H6S 0.9500 . ?
C6S C5S 1.3895 . ?
C5S H5S 0.9500 . ?
C5S C4S 1.3815 . ?
C4S H4S 0.9500 . ?
C4S C3S 1.3799 . ?
C3S H3S 0.9500 . ?
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
C1 C2 C3 C5 -142.8(6) . . . . ?
C1 C2 C3 C4 106.6(6) . . . . ?
C1 C2 C4 C3 -104.1(6) . . . . ?
C1 C2 C11 C12 75.2(7) . . . . ?
C1 C2 C11 C16 -100.6(7) . . . . ?
C25 C24 C23 C22 -0.8(16) . . . . ?
C25 C26 C21 C19 179.0(9) . . . . ?
C25 C26 C21 C22 -1.1(13) . . . . ?
C2 C1 O1 Rh1 175.8(4) . . . . ?
C2 C1 O2 Rh1 -173.0(4) . . . 2_665 ?
C2 C3 C5 C6 -47.1(10) . . . . ?
C2 C3 C5 C10 135.8(7) . . . . ?
C2 C11 C12 C13 -174.4(6) . . . . ?
C2 C11 C16 C15 174.0(6) . . . . ?
O1 C1 C2 C3 -38.9(8) . . . . ?
O1 C1 C2 C4 26.7(8) . . . . ?
O1 C1 C2 C11 175.4(6) . . . . ?
O1 C1 O2 Rh1 8.1(9) . . . 2_665 ?
C3 C2 C11 C12 -67.9(9) . . . . ?
C3 C2 C11 C16 116.3(7) . . . . ?
C3 C5 C6 C7 -178.3(8) . . . . ?
C3 C5 C10 C9 176.7(7) . . . . ?
C5 C3 C4 C2 -110.4(7) . . . . ?
C4 C2 C3 C5 110.6(7) . . . . ?
C4 C2 C11 C12 -138.2(6) . . . . ?
C4 C2 C11 C16 46.0(8) . . . . ?
C4 C3 C5 C6 23.5(10) . . . . ?
C4 C3 C5 C10 -153.6(7) . . . . ?
C27 C18 C19 C20 -113.0(7) . . . . ?
C27 C18 C19 C21 -1.5(10) . . . . ?
C27 C18 C20 C19 102.8(7) . . . . ?
C7 C8 C9 C10 -1.1(13) . . . . ?
C8 C7 C6 C5 1.7(15) . . . . ?
C8 C9 C10 C5 1.7(12) . . . . ?
O3 C17 O4 Rh1 8.5(8) . . . 2_665 ?
O3 C17 C18 C27 -171.4(6) . . . . ?
O3 C17 C18 C19 -29.4(8) . . . . ?
O3 C17 C18 C20 34.4(8) . . . . ?
C6 C5 C10 C9 -0.5(11) . . . . ?
C6 C7 C8 C9 -0.5(15) . . . . ?
Rh1 O3 C17 O4 -6.5(8) . . . . ?
Rh1 O3 C17 C18 176.0(4) . . . . ?
C11 C2 C3 C5 0.1(11) . . . . ?
C11 C2 C3 C4 -110.6(8) . . . . ?
C11 C2 C4 C3 109.9(6) . . . . ?
C11 C12 C13 C14 -0.5(9) . . . . ?
C24 C25 C26 C21 -1.3(16) . . . . ?
C12 C11 C16 C15 -1.8(10) . . . . ?
C12 C13 C14 C15 0.0(10) . . . . ?
C26 C25 C24 C23 2.3(17) . . . . ?
C26 C21 C22 C23 2.6(12) . . . . ?
C13 C14 C15 C16 -0.4(11) . . . . ?
C28 C29 C30 C31 -0.7(16) . . . . ?
C28 C27 C32 C31 3.0(14) . . . . ?
C28 C27 C18 C17 51.5(8) . . . . ?
C28 C27 C18 C19 -89.8(8) . . . . ?
C28 C27 C18 C20 -156.4(7) . . . . ?
C14 C15 C16 C11 1.3(11) . . . . ?
C30 C29 C28 C27 -0.1(13) . . . . ?
C30 C31 C32 C27 -4.0(19) . . . . ?
C32 C27 C28 C29 -1.0(11) . . . . ?
C32 C27 C18 C17 -134.9(8) . . . . ?
C32 C27 C18 C19 83.8(10) . . . . ?
C32 C27 C18 C20 17.1(11) . . . . ?
C32 C31 C30 C29 2.7(19) . . . . ?
C16 C11 C12 C13 1.5(9) . . . . ?
O2 C1 C2 C3 142.1(6) . . . . ?
O2 C1 C2 C4 -152.3(6) . . . . ?
O2 C1 C2 C11 -3.6(8) . . . . ?
O2 C1 O1 Rh1 -5.4(9) . . . . ?
C17 C18 C19 C20 104.5(6) . . . . ?
C17 C18 C19 C21 -144.0(6) . . . . ?
C17 C18 C20 C19 -104.4(6) . . . . ?
O4 C17 C18 C27 10.9(9) . . . . ?
O4 C17 C18 C19 153.0(6) . . . . ?
O4 C17 C18 C20 -143.3(6) . . . . ?
C18 C27 C28 C29 172.8(7) . . . . ?
C18 C27 C32 C31 -170.8(9) . . . . ?
C18 C17 O4 Rh1 -174.0(4) . . . 2_665 ?
C18 C19 C21 C26 -97.0(9) . . . . ?
C18 C19 C21 C22 83.1(9) . . . . ?
C10 C5 C6 C7 -1.2(13) . . . . ?
C19 C21 C22 C23 -177.5(7) . . . . ?
C8S C9S C14S C13S 179.6(15) . . . . ?
C8S C9S C10S C11S 177.8(15) . . . . ?
C20 C18 C19 C21 111.5(8) . . . . ?
C20 C19 C21 C26 -26.8(10) . . . . ?
C20 C19 C21 C22 153.2(7) . . . . ?
C14S C9S C10S C11S -3(3) . . . . ?
C14S C13S C12S C11S -2(2) . . . . ?
C21 C19 C20 C18 -107.0(7) . . . . ?
C21 C22 C23 C24 -1.6(14) . . . . ?
C12S C11S C10S C9S 3(2) . . . . ?
C12S C13S C14S C9S 2(2) . . . . ?
C10S C9S C14S C13S 1(2) . . . . ?
C10S C11S C12S C13S -1(2) . . . . ?
C1S' C2S' C7S' C6S' -179(2) . . . . ?
C1S' C2S' C3S' C4S' -178(2) . . . . ?
C2S' C7S' C6S' C5S' -1(5) . . . . ?
C7S' C2S' C3S' C4S' 3(4) . . . . ?
C7S' C6S' C5S' C4S' -1(7) . . . . ?
C6S' C5S' C4S' C3S' 4(7) . . . . ?
C5S' C4S' C3S' C2S' -5(5) . . . . ?
C3S' C2S' C7S' C6S' 0(4) . . . . ?
C1S C2S C7S C6S -179.7 . . . . ?
C1S C2S C3S C4S 179.8 . . . . ?
C2S C7S C6S C5S 0.1 . . . . ?
C7S C2S C3S C4S 0.2 . . . . ?
C7S C6S C5S C4S -0.3 . . . . ?
C6S C5S C4S C3S 0.4 . . . . ?
C5S C4S C3S C2S -0.3 . . . . ?
C3S C2S C7S C6S -0.1 . . . . ?
