#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:16:28 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180032 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/26/7032647.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_7032647
loop_
_publ_author_name
'Shen, Xu-Yu'
'Zhang, Long'
'Lin, Yue-Jian'
'Jin, Guo-Xin'
_publ_section_title
;
 Construction of iridium and rhodium cyclometalated macrocycles based on
 p-carborane and N,N'-donor bridging ligands.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17200
_journal_page_last               17208
_journal_paper_doi               10.1039/c4dt02495h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C38 H44 Cl2 N4 Rh2, 2(C F3 O3 S)'
_chemical_formula_sum            'C40 H44 Cl2 F6 N4 O6 Rh2 S2'
_chemical_formula_weight         1131.63
_chemical_name_systematic        2b
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90.0310(10)
_cell_angle_beta                 95.8710(10)
_cell_angle_gamma                91.7070(10)
_cell_formula_units_Z            1
_cell_length_a                   8.9099(7)
_cell_length_b                   10.7092(8)
_cell_length_c                   11.8825(9)
_cell_measurement_reflns_used    4512
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.56
_cell_volume                     1127.35(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8328
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         1.723
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_description       block
_exptl_crystal_F_000             570
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.651
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5089
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0347
_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)+(0.0472P)²+2.2656P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0865
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4518
_reflns_number_total             5089
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4dt02495h1.cif
_cod_data_source_block           2b
_cod_depositor_comments
'Adding full bibliography for 7032645--7032650.cif.'
_cod_database_code               7032647
#BEGIN Tags that were not found in dictionaries:
_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   0.923
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
Rh1 Rh 0.63743(3) 0.78194(2) 0.81349(2) 0.01976(9) Uani 1 1 d . .
Cl1 Cl 0.49154(12) 0.77201(10) 0.97163(8) 0.0417(2) Uani 1 1 d . .
N1 N 0.7229(3) 0.9608(3) 0.8687(2) 0.0219(5) Uani 1 1 d . .
N2 N 0.4764(3) 0.9057(3) 0.7379(2) 0.0240(6) Uani 1 1 d . .
O1 O 0.0946(4) 0.8380(3) 0.3754(3) 0.0441(7) Uani 1 1 d . .
O2 O 0.2014(4) 0.6712(3) 0.4904(3) 0.0550(9) Uani 1 1 d . .
O3 O 0.2585(4) 0.6921(4) 0.2963(4) 0.0690(11) Uani 1 1 d . .
S1 S 0.15672(10) 0.71572(10) 0.37907(8) 0.0347(2) Uani 1 1 d . .
F1 F 0.0244(4) 0.4960(3) 0.3371(3) 0.0652(9) Uani 1 1 d . .
F2 F -0.1181(3) 0.6298(3) 0.3988(3) 0.0590(8) Uani 1 1 d . .
F3 F -0.0627(5) 0.6429(4) 0.2284(3) 0.0906(13) Uani 1 1 d . .
C1 C 0.8851(4) 0.9281(3) 1.0425(3) 0.0270(7) Uani 1 1 d . .
H1 H 0.8066 0.8788 1.0704 0.032 Uiso 1 1 calc R U
C2 C 0.8637(4) 0.9828(3) 0.9359(3) 0.0221(6) Uani 1 1 d . .
C3 C 0.9775(4) 1.0535(3) 0.8927(3) 0.0257(7) Uani 1 1 d . .
H3 H 0.9614 1.0890 0.8194 0.031 Uiso 1 1 calc R U
C4 C 0.6454(4) 1.0534(3) 0.8349(3) 0.0247(7) Uani 1 1 d . .
H4 H 0.6782 1.1365 0.8548 0.030 Uiso 1 1 calc R U
C5 C 0.5038(4) 1.0277(3) 0.7642(3) 0.0247(7) Uani 1 1 d . .
C6 C 0.4044(4) 1.1196(3) 0.7280(3) 0.0314(8) Uani 1 1 d . .
H6 H 0.4252 1.2044 0.7491 0.038 Uiso 1 1 calc R U
C7 C 0.2743(4) 1.0853(4) 0.6605(3) 0.0335(8) Uani 1 1 d . .
H7 H 0.2036 1.1462 0.6345 0.040 Uiso 1 1 calc R U
C8 C 0.2486(4) 0.9619(4) 0.6315(3) 0.0327(8) Uani 1 1 d . .
H8 H 0.1617 0.9371 0.5827 0.039 Uiso 1 1 calc R U
C9 C 0.3497(4) 0.8739(4) 0.6735(3) 0.0307(7) Uani 1 1 d . .
H9 H 0.3283 0.7882 0.6560 0.037 Uiso 1 1 calc R U
C10 C 0.7235(4) 0.5947(3) 0.8437(3) 0.0308(7) Uani 1 1 d . .
C11 C 0.6076(4) 0.5942(3) 0.7498(3) 0.0281(7) Uani 1 1 d . .
C12 C 0.6612(4) 0.6716(3) 0.6633(3) 0.0260(7) Uani 1 1 d . .
C13 C 0.8028(4) 0.7277(3) 0.7063(3) 0.0276(7) Uani 1 1 d . .
C14 C 0.8432(4) 0.6761(3) 0.8175(3) 0.0280(7) Uani 1 1 d . .
C15 C 0.7196(6) 0.5182(5) 0.9477(4) 0.0538(12) Uani 1 1 d . .
H15A H 0.7454 0.4321 0.9316 0.081 Uiso 1 1 calc R U
H15B H 0.6181 0.5188 0.9727 0.081 Uiso 1 1 calc R U
H15C H 0.7927 0.5532 1.0076 0.081 Uiso 1 1 calc R U
C16 C 0.4648(5) 0.5154(4) 0.7406(4) 0.0464(11) Uani 1 1 d . .
H16A H 0.4853 0.4317 0.7139 0.070 Uiso 1 1 calc R U
H16B H 0.3890 0.5538 0.6869 0.070 Uiso 1 1 calc R U
H16C H 0.4268 0.5094 0.8150 0.070 Uiso 1 1 calc R U
C17 C 0.5840(5) 0.6901(5) 0.5475(3) 0.0431(10) Uani 1 1 d . .
H17A H 0.5992 0.7770 0.5245 0.065 Uiso 1 1 calc R U
H17B H 0.4758 0.6711 0.5477 0.065 Uiso 1 1 calc R U
H17C H 0.6263 0.6343 0.4943 0.065 Uiso 1 1 calc R U
C18 C 0.9004(5) 0.8134(4) 0.6447(4) 0.0418(10) Uani 1 1 d . .
H18A H 0.9684 0.7643 0.6037 0.063 Uiso 1 1 calc R U
H18B H 0.9600 0.8688 0.6990 0.063 Uiso 1 1 calc R U
H18C H 0.8370 0.8635 0.5909 0.063 Uiso 1 1 calc R U
C19 C 0.9920(5) 0.6965(4) 0.8862(4) 0.0452(11) Uani 1 1 d . .
H19A H 0.9836 0.6698 0.9642 0.068 Uiso 1 1 calc R U
H19B H 1.0214 0.7854 0.8856 0.068 Uiso 1 1 calc R U
H19C H 1.0685 0.6477 0.8539 0.068 Uiso 1 1 calc R U
C20 C -0.0075(5) 0.6144(4) 0.3333(4) 0.0406(9) Uani 1 1 d . .
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
N2 Rh1 N1 76.11(11) .
N2 Rh1 C13 114.51(13) .
N1 Rh1 C13 101.42(12) .
N2 Rh1 C11 113.57(13) .
N1 Rh1 C11 165.82(12) .
C13 Rh1 C11 65.50(14) .
N2 Rh1 C12 97.11(12) .
N1 Rh1 C12 132.89(12) .
C13 Rh1 C12 38.67(13) .
C11 Rh1 C12 38.70(13) .
N2 Rh1 C14 153.35(13) .
N1 Rh1 C14 101.84(12) .
C13 Rh1 C14 39.16(14) .
C11 Rh1 C14 64.73(13) .
C12 Rh1 C14 64.39(13) .
N2 Rh1 C10 151.86(13) .
N1 Rh1 C10 132.02(13) .
C13 Rh1 C10 64.85(14) .
C11 Rh1 C10 38.83(14) .
C12 Rh1 C10 64.25(14) .
C14 Rh1 C10 37.89(14) .
N2 Rh1 Cl1 87.30(8) .
N1 Rh1 Cl1 89.37(8) .
C13 Rh1 Cl1 157.33(11) .
C11 Rh1 Cl1 101.11(10) .
C12 Rh1 Cl1 137.41(10) .
C14 Rh1 Cl1 119.35(10) .
C10 Rh1 Cl1 93.09(10) .
C4 N1 C2 119.0(3) .
C4 N1 Rh1 116.7(2) .
C2 N1 Rh1 124.3(2) .
C9 N2 C5 118.4(3) .
C9 N2 Rh1 126.3(2) .
C5 N2 Rh1 115.2(2) .
O2 S1 O3 115.7(2) .
O2 S1 O1 114.5(2) .
O3 S1 O1 115.4(2) .
O2 S1 C20 102.6(2) .
O3 S1 C20 103.1(2) .
O1 S1 C20 102.84(19) .
C3 C1 C2 119.1(3) 2_777
C3 C2 C1 121.4(3) .
C3 C2 N1 119.9(3) .
C1 C2 N1 118.6(3) .
C1 C3 C2 119.5(3) 2_777
N1 C4 C5 117.5(3) .
N2 C5 C6 122.4(3) .
N2 C5 C4 114.4(3) .
C6 C5 C4 123.2(3) .
C7 C6 C5 118.5(3) .
C8 C7 C6 119.0(3) .
C7 C8 C9 119.7(3) .
N2 C9 C8 121.9(4) .
C14 C10 C11 108.3(3) .
C14 C10 C15 126.3(4) .
C11 C10 C15 125.4(4) .
C14 C10 Rh1 70.9(2) .
C11 C10 Rh1 69.1(2) .
C15 C10 Rh1 127.6(3) .
C12 C11 C10 107.6(3) .
C12 C11 C16 126.6(4) .
C10 C11 C16 125.5(4) .
C12 C11 Rh1 71.60(19) .
C10 C11 Rh1 72.0(2) .
C16 C11 Rh1 126.8(3) .
C13 C12 C11 108.3(3) .
C13 C12 C17 125.5(3) .
C11 C12 C17 126.2(3) .
C13 C12 Rh1 69.30(19) .
C11 C12 Rh1 69.70(19) .
C17 C12 Rh1 127.1(3) .
C12 C13 C14 107.6(3) .
C12 C13 C18 126.8(3) .
C14 C13 C18 125.4(3) .
C12 C13 Rh1 72.03(19) .
C14 C13 Rh1 72.06(19) .
C18 C13 Rh1 126.2(3) .
C10 C14 C13 108.0(3) .
C10 C14 C19 126.5(4) .
C13 C14 C19 125.2(4) .
C10 C14 Rh1 71.2(2) .
C13 C14 Rh1 68.78(19) .
C19 C14 Rh1 130.0(3) .
F1 C20 F2 107.0(4) .
F1 C20 F3 109.0(4) .
F2 C20 F3 106.8(4) .
F1 C20 S1 112.3(3) .
F2 C20 S1 111.1(3) .
F3 C20 S1 110.4(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N2 2.115(3) .
Rh1 N1 2.119(3) .
Rh1 C13 2.136(3) .
Rh1 C11 2.147(3) .
Rh1 C12 2.172(3) .
Rh1 C14 2.180(3) .
Rh1 C10 2.186(4) .
Rh1 Cl1 2.3924(9) .
N1 C4 1.267(4) .
N1 C2 1.429(4) .
N2 C9 1.333(4) .
N2 C5 1.353(4) .
O1 S1 1.435(3) .
O2 S1 1.429(3) .
O3 S1 1.432(4) .
S1 C20 1.832(4) .
F1 C20 1.309(5) .
F2 C20 1.330(5) .
F3 C20 1.331(5) .
C1 C3 1.387(5) 2_777
C1 C2 1.394(5) .
C2 C3 1.388(5) .
C3 C1 1.387(5) 2_777
C4 C5 1.462(5) .
C5 C6 1.382(5) .
C6 C7 1.381(5) .
C7 C8 1.371(6) .
C8 C9 1.382(5) .
C10 C14 1.417(5) .
C10 C11 1.441(5) .
C10 C15 1.486(6) .
C11 C12 1.432(5) .
C11 C16 1.500(5) .
C12 C13 1.427(5) .
C12 C17 1.489(5) .
C13 C14 1.447(5) .
C13 C18 1.490(5) .
C14 C19 1.494(5) .
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_4
C3 C1 C2 C3 1.0(6) 2_777 .
C3 C1 C2 N1 178.5(3) 2_777 .
C4 N1 C2 C3 -59.7(4) . .
Rh1 N1 C2 C3 117.0(3) . .
C4 N1 C2 C1 122.7(4) . .
Rh1 N1 C2 C1 -60.5(4) . .
C1 C2 C3 C1 -1.0(6) . 2_777
N1 C2 C3 C1 -178.5(3) . 2_777
C2 N1 C4 C5 178.6(3) . .
Rh1 N1 C4 C5 1.6(4) . .
C9 N2 C5 C6 0.9(5) . .
Rh1 N2 C5 C6 -175.6(3) . .
C9 N2 C5 C4 -179.9(3) . .
Rh1 N2 C5 C4 3.6(4) . .
N1 C4 C5 N2 -3.5(5) . .
N1 C4 C5 C6 175.7(3) . .
N2 C5 C6 C7 -1.5(6) . .
C4 C5 C6 C7 179.4(3) . .
C5 C6 C7 C8 -0.2(6) . .
C6 C7 C8 C9 2.4(6) . .
C5 N2 C9 C8 1.4(5) . .
Rh1 N2 C9 C8 177.5(3) . .
C7 C8 C9 N2 -3.1(6) . .
C14 C10 C11 C12 2.9(4) . .
C15 C10 C11 C12 -174.8(4) . .
Rh1 C10 C11 C12 63.2(2) . .
C14 C10 C11 C16 176.8(4) . .
C15 C10 C11 C16 -0.8(6) . .
Rh1 C10 C11 C16 -122.9(4) . .
C14 C10 C11 Rh1 -60.3(2) . .
C15 C10 C11 Rh1 122.0(4) . .
C10 C11 C12 C13 -4.8(4) . .
C16 C11 C12 C13 -178.6(4) . .
Rh1 C11 C12 C13 58.7(2) . .
C10 C11 C12 C17 174.7(4) . .
C16 C11 C12 C17 0.9(6) . .
Rh1 C11 C12 C17 -121.8(4) . .
C10 C11 C12 Rh1 -63.5(2) . .
C16 C11 C12 Rh1 122.7(4) . .
C11 C12 C13 C14 4.8(4) . .
C17 C12 C13 C14 -174.7(4) . .
Rh1 C12 C13 C14 63.7(2) . .
C11 C12 C13 C18 178.9(4) . .
C17 C12 C13 C18 -0.7(6) . .
Rh1 C12 C13 C18 -122.2(4) . .
C11 C12 C13 Rh1 -59.0(2) . .
C17 C12 C13 Rh1 121.5(4) . .
C11 C10 C14 C13 0.1(4) . .
C15 C10 C14 C13 177.7(4) . .
Rh1 C10 C14 C13 -59.2(2) . .
C11 C10 C14 C19 -174.3(3) . .
C15 C10 C14 C19 3.3(6) . .
Rh1 C10 C14 C19 126.4(4) . .
C11 C10 C14 Rh1 59.2(2) . .
C15 C10 C14 Rh1 -123.1(4) . .
C12 C13 C14 C10 -3.0(4) . .
C18 C13 C14 C10 -177.2(4) . .
Rh1 C13 C14 C10 60.7(2) . .
C12 C13 C14 C19 171.5(3) . .
C18 C13 C14 C19 -2.7(6) . .
Rh1 C13 C14 C19 -124.8(4) . .
C12 C13 C14 Rh1 -63.7(2) . .
C18 C13 C14 Rh1 122.1(4) . .
O2 S1 C20 F1 -57.2(4) . .
O3 S1 C20 F1 63.3(4) . .
O1 S1 C20 F1 -176.3(3) . .
O2 S1 C20 F2 62.6(4) . .
O3 S1 C20 F2 -176.8(3) . .
O1 S1 C20 F2 -56.5(4) . .
O2 S1 C20 F3 -179.1(3) . .
O3 S1 C20 F3 -58.5(4) . .
O1 S1 C20 F3 61.8(4) . .
