#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:56:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179270 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/90/4319062.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_4319062
loop_
_publ_author_name
'Chayan Das'
'Amit K. Ghosh'
'Chen-Hsiung Hung'
'Gene-Hsiang Lee'
'Shie-Ming Peng'
'Sreebrata Goswami'
_publ_section_title
;
 Metal-Promoted Aromatic Ring Amination and Deamination Reactions at a
 Diazo Ligand Coordinated to Rhodium and Ruthenium
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7125
_journal_page_last               7135
_journal_paper_doi               10.1021/ic020421c
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C36 H31 Cl F6 N8 P Rh'
_chemical_formula_weight         859.02
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.483(2)
_cell_angle_beta                 104.519(2)
_cell_angle_gamma                92.834(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9645(8)
_cell_length_b                   12.4699(12)
_cell_length_c                   17.0283(17)
_cell_measurement_temperature    293(2)
_cell_volume                     1741.5(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_sigmaI/netI    0.2171
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11255
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7299
_exptl_absorpt_correction_type   'Empirical Used SADABS'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'Thin Plate'
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.793
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         7761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.1160
_refine_ls_R_factor_gt           0.0506
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0692P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1071
_refine_ls_wR_factor_ref         0.1769
_reflns_number_gt                3301
_reflns_number_total             7761
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020421c_5.cif
_cod_data_source_block           '[RhCl(HL2b)(L1b)]PF6,(6d)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4319062
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.80118(7) 0.80119(5) 0.66743(4) 0.02689(18) Uani 1 1 d . . .
Cl1 Cl 0.62119(19) 0.65555(14) 0.55980(11) 0.0306(4) Uani 1 1 d . . .
N1 N 0.6493(6) 0.9177(4) 0.6649(4) 0.0279(14) Uani 1 1 d . . .
N2 N 0.8487(6) 0.8508(4) 0.5779(4) 0.0262(14) Uani 1 1 d . . .
N3 N 0.9440(7) 0.7996(5) 0.5363(4) 0.0312(15) Uani 1 1 d . . .
N4 N 0.9746(6) 0.7067(4) 0.6427(4) 0.0264(14) Uani 1 1 d . . .
N5 N 0.7562(6) 0.7524(4) 0.7652(4) 0.0284(14) Uani 1 1 d . . .
N6 N 0.9187(7) 0.9254(5) 0.8477(4) 0.0310(14) Uani 1 1 d . . .
N7 N 0.9313(6) 0.9280(5) 0.7751(4) 0.0289(14) Uani 1 1 d . . .
N8 N 1.2701(7) 1.3330(5) 0.8113(5) 0.054(2) Uani 1 1 d . . .
H8A H 1.2461 1.3945 0.8420 0.065 Uiso 1 1 calc R . .
C1 C 0.3422(9) 1.0142(7) 0.9277(5) 0.054(3) Uani 1 1 d . . .
H1A H 0.2418 1.0363 0.9087 0.081 Uiso 1 1 calc R . .
H1B H 0.4055 1.0747 0.9762 0.081 Uiso 1 1 calc R . .
H1C H 0.3303 0.9475 0.9438 0.081 Uiso 1 1 calc R . .
C2 C 0.4171(8) 0.9900(7) 0.8579(5) 0.0357(19) Uani 1 1 d . . .
C3 C 0.5229(8) 1.0750(6) 0.8536(5) 0.037(2) Uani 1 1 d . . .
H3 H 0.5449 1.1459 0.8956 0.045 Uiso 1 1 calc R . .
C4 C 0.5936(8) 1.0548(6) 0.7885(5) 0.0335(19) Uani 1 1 d . . .
H4 H 0.6626 1.1119 0.7870 0.040 Uiso 1 1 calc R . .
C5 C 0.5625(8) 0.9498(6) 0.7252(5) 0.0287(17) Uani 1 1 d . . .
C6 C 0.4563(8) 0.8650(6) 0.7276(5) 0.0280(17) Uani 1 1 d . . .
H6 H 0.4338 0.7945 0.6851 0.034 Uiso 1 1 calc R . .
C7 C 0.3846(8) 0.8856(6) 0.7933(5) 0.0363(19) Uani 1 1 d . . .
H7 H 0.3141 0.8289 0.7940 0.044 Uiso 1 1 calc R . .
C8 C 0.6761(8) 0.9774(6) 0.6138(5) 0.0315(18) Uani 1 1 d . . .
C9 C 0.6059(8) 1.0761(6) 0.6054(5) 0.0358(19) Uani 1 1 d . . .
H9 H 0.5425 1.1073 0.6396 0.043 Uiso 1 1 calc R . .
C10 C 0.6324(8) 1.1230(6) 0.5481(5) 0.038(2) Uani 1 1 d . . .
H10 H 0.5880 1.1878 0.5446 0.046 Uiso 1 1 calc R . .
C11 C 0.7263(8) 1.0776(6) 0.4916(5) 0.0375(19) Uani 1 1 d . . .
H11 H 0.7370 1.1101 0.4504 0.045 Uiso 1 1 calc R . .
C12 C 0.7989(8) 0.9869(6) 0.4994(5) 0.0328(18) Uani 1 1 d . . .
H12 H 0.8626 0.9577 0.4649 0.039 Uiso 1 1 calc R . .
C13 C 0.7758(8) 0.9371(6) 0.5615(5) 0.0274(17) Uani 1 1 d . . .
C14 C 1.0109(8) 0.7214(5) 0.5715(5) 0.0278(17) Uani 1 1 d . . .
C15 C 1.1168(8) 0.6576(6) 0.5369(5) 0.0337(19) Uani 1 1 d . . .
H15 H 1.1389 0.6650 0.4881 0.040 Uiso 1 1 calc R . .
C16 C 1.1885(8) 0.5839(6) 0.5753(5) 0.038(2) Uani 1 1 d . . .
H16 H 1.2603 0.5423 0.5530 0.045 Uiso 1 1 calc R . .
C17 C 1.1529(9) 0.5716(6) 0.6479(5) 0.043(2) Uani 1 1 d . . .
H17 H 1.2012 0.5227 0.6749 0.052 Uiso 1 1 calc R . .
C18 C 1.0450(8) 0.6336(6) 0.6785(5) 0.0320(18) Uani 1 1 d . . .
H18 H 1.0196 0.6245 0.7260 0.038 Uiso 1 1 calc R . .
C19 C 0.6610(8) 0.6643(6) 0.7631(5) 0.0360(19) Uani 1 1 d . . .
H19 H 0.6108 0.6110 0.7101 0.043 Uiso 1 1 calc R . .
C20 C 0.6341(10) 0.6489(7) 0.8342(5) 0.044(2) Uani 1 1 d . . .
H20 H 0.5678 0.5860 0.8293 0.052 Uiso 1 1 calc R . .
C21 C 0.7039(10) 0.7250(7) 0.9122(6) 0.044(2) Uani 1 1 d . . .
H21 H 0.6844 0.7160 0.9611 0.053 Uiso 1 1 calc R . .
C22 C 0.8060(9) 0.8174(7) 0.9182(5) 0.042(2) Uani 1 1 d . . .
H22 H 0.8601 0.8691 0.9712 0.051 Uiso 1 1 calc R . .
C23 C 0.8239(8) 0.8295(6) 0.8439(5) 0.0318(18) Uani 1 1 d . . .
C24 C 1.0082(8) 1.0319(6) 0.7768(5) 0.0319(18) Uani 1 1 d . . .
C25 C 1.0972(7) 1.0338(6) 0.7230(4) 0.0275(17) Uani 1 1 d . . .
H25 H 1.0989 0.9679 0.6796 0.033 Uiso 1 1 calc R . .
C26 C 1.1854(8) 1.1339(6) 0.7329(5) 0.0309(18) Uani 1 1 d . . .
H26 H 1.2485 1.1347 0.6972 0.037 Uiso 1 1 calc R . .
C27 C 1.1792(8) 1.2342(6) 0.7970(5) 0.0348(19) Uani 1 1 d . . .
C28 C 1.0798(8) 1.2338(6) 0.8467(5) 0.041(2) Uani 1 1 d . . .
H28 H 1.0687 1.3018 0.8851 0.049 Uiso 1 1 calc R . .
C29 C 0.9965(8) 1.1350(6) 0.8409(5) 0.0365(19) Uani 1 1 d . . .
H29 H 0.9345 1.1345 0.8772 0.044 Uiso 1 1 calc R . .
C30 C 1.4023(10) 1.3432(6) 0.7795(5) 0.037(2) Uani 1 1 d . . .
C31 C 1.3844(10) 1.3423(6) 0.6946(6) 0.046(2) Uani 1 1 d . . .
H31 H 1.2861 1.3306 0.6563 0.055 Uiso 1 1 calc R . .
C32 C 1.5153(11) 1.3591(6) 0.6702(5) 0.043(2) Uani 1 1 d . . .
H32 H 1.5044 1.3607 0.6148 0.052 Uiso 1 1 calc R . .
C33 C 1.6625(9) 1.3738(6) 0.7243(6) 0.041(2) Uani 1 1 d . . .
C34 C 1.6810(10) 1.3745(6) 0.8061(5) 0.043(2) Uani 1 1 d . . .
H34 H 1.7799 1.3846 0.8434 0.052 Uiso 1 1 calc R . .
C35 C 1.5503(9) 1.3600(6) 0.8330(5) 0.042(2) Uani 1 1 d . . .
H35 H 1.5631 1.3618 0.8893 0.050 Uiso 1 1 calc R . .
C36 C 1.8059(11) 1.3922(7) 0.6948(6) 0.069(3) Uani 1 1 d . . .
H36A H 1.8460 1.3215 0.6774 0.103 Uiso 1 1 calc R . .
H36B H 1.8840 1.4461 0.7411 0.103 Uiso 1 1 calc R . .
H36C H 1.7783 1.4206 0.6473 0.103 Uiso 1 1 calc R . .
F1 F 0.0186(6) 0.5867(5) 0.8817(4) 0.096(2) Uani 1 1 d . . .
F2 F 0.2377(6) 0.5772(4) 0.8385(3) 0.0637(15) Uani 1 1 d . . .
F3 F 0.2274(7) 0.5320(4) 0.9548(3) 0.0758(17) Uani 1 1 d . . .
F4 F 0.1555(6) 0.7005(4) 1.0121(3) 0.0643(15) Uani 1 1 d . . .
F5 F 0.1621(7) 0.7461(4) 0.8936(4) 0.0783(17) Uani 1 1 d . . .
F6 F 0.3707(5) 0.6918(5) 0.9676(3) 0.0739(17) Uani 1 1 d . . .
P1 P 0.1952(3) 0.64055(18) 0.92461(14) 0.0418(6) 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
N2 Rh1 N1 82.0(2) . . ?
N2 Rh1 N4 79.4(2) . . ?
N1 Rh1 N4 161.2(2) . . ?
N2 Rh1 N5 178.2(2) . . ?
N1 Rh1 N5 98.1(2) . . ?
N4 Rh1 N5 100.5(2) . . ?
N2 Rh1 N7 101.0(2) . . ?
N1 Rh1 N7 83.0(2) . . ?
N4 Rh1 N7 98.4(2) . . ?
N5 Rh1 N7 77.3(2) . . ?
N2 Rh1 Cl1 88.00(16) . . ?
N1 Rh1 Cl1 92.82(16) . . ?
N4 Rh1 Cl1 88.64(16) . . ?
N5 Rh1 Cl1 93.79(17) . . ?
N7 Rh1 Cl1 169.43(17) . . ?
C8 N1 C5 125.4(6) . . ?
C8 N1 Rh1 109.4(4) . . ?
C5 N1 Rh1 123.1(5) . . ?
N3 N2 C13 124.1(6) . . ?
N3 N2 Rh1 120.2(4) . . ?
C13 N2 Rh1 115.7(5) . . ?
N2 N3 C14 111.3(6) . . ?
C18 N4 C14 119.4(6) . . ?
C18 N4 Rh1 131.9(5) . . ?
C14 N4 Rh1 108.6(4) . . ?
C19 N5 C23 116.0(7) . . ?
C19 N5 Rh1 130.7(5) . . ?
C23 N5 Rh1 112.9(5) . . ?
N7 N6 C23 114.7(6) . . ?
N6 N7 C24 115.0(6) . . ?
N6 N7 Rh1 117.6(5) . . ?
C24 N7 Rh1 126.0(5) . . ?
C27 N8 C30 125.7(6) . . ?
C7 C2 C3 117.9(7) . . ?
C7 C2 C1 121.8(8) . . ?
C3 C2 C1 120.3(7) . . ?
C4 C3 C2 121.4(7) . . ?
C3 C4 C5 120.3(7) . . ?
C4 C5 C6 119.2(7) . . ?
C4 C5 N1 122.9(6) . . ?
C6 C5 N1 117.3(6) . . ?
C7 C6 C5 120.5(7) . . ?
C2 C7 C6 120.8(7) . . ?
N1 C8 C13 117.9(6) . . ?
N1 C8 C9 125.1(7) . . ?
C13 C8 C9 116.9(7) . . ?
C10 C9 C8 119.7(7) . . ?
C9 C10 C11 123.2(7) . . ?
C12 C11 C10 119.0(7) . . ?
C11 C12 C13 118.9(7) . . ?
N2 C13 C8 113.9(6) . . ?
N2 C13 C12 123.8(6) . . ?
C8 C13 C12 122.2(6) . . ?
N3 C14 N4 119.8(6) . . ?
N3 C14 C15 120.5(7) . . ?
N4 C14 C15 119.6(7) . . ?
C16 C15 C14 119.9(7) . . ?
C15 C16 C17 119.8(7) . . ?
C18 C17 C16 118.5(7) . . ?
N4 C18 C17 122.8(7) . . ?
N5 C19 C20 123.5(8) . . ?
C21 C20 C19 119.9(8) . . ?
C20 C21 C22 119.0(8) . . ?
C23 C22 C21 117.9(8) . . ?
N5 C23 C22 123.5(7) . . ?
N5 C23 N6 117.3(7) . . ?
C22 C23 N6 119.2(7) . . ?
C25 C24 N7 121.5(6) . . ?
C25 C24 C29 120.6(7) . . ?
N7 C24 C29 117.9(6) . . ?
C24 C25 C26 120.1(7) . . ?
C25 C26 C27 119.9(7) . . ?
N8 C27 C28 118.8(7) . . ?
N8 C27 C26 121.4(7) . . ?
C28 C27 C26 119.8(7) . . ?
C29 C28 C27 121.4(7) . . ?
C28 C29 C24 117.9(7) . . ?
C35 C30 C31 118.3(7) . . ?
C35 C30 N8 120.3(8) . . ?
C31 C30 N8 121.3(8) . . ?
C32 C31 C30 118.2(8) . . ?
C31 C32 C33 122.6(8) . . ?
C34 C33 C32 119.6(8) . . ?
C34 C33 C36 119.2(8) . . ?
C32 C33 C36 121.2(9) . . ?
C33 C34 C35 118.9(8) . . ?
C30 C35 C34 122.3(8) . . ?
F6 P1 F5 90.7(3) . . ?
F6 P1 F1 178.9(4) . . ?
F5 P1 F1 90.4(4) . . ?
F6 P1 F4 90.2(3) . . ?
F5 P1 F4 91.6(3) . . ?
F1 P1 F4 89.8(3) . . ?
F6 P1 F2 89.2(3) . . ?
F5 P1 F2 90.4(3) . . ?
F1 P1 F2 90.7(3) . . ?
F4 P1 F2 177.9(3) . . ?
F6 P1 F3 89.9(3) . . ?
F5 P1 F3 179.2(3) . . ?
F1 P1 F3 89.0(3) . . ?
F4 P1 F3 89.0(3) . . ?
F2 P1 F3 89.0(3) . . ?
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 N2 1.937(6) . ?
Rh1 N1 2.042(5) . ?
Rh1 N4 2.048(5) . ?
Rh1 N5 2.055(6) . ?
Rh1 N7 2.056(6) . ?
Rh1 Cl1 2.3427(18) . ?
N1 C8 1.359(9) . ?
N1 C5 1.415(8) . ?
N2 N3 1.313(7) . ?
N2 C13 1.351(8) . ?
N3 C14 1.378(9) . ?
N4 C18 1.341(8) . ?
N4 C14 1.391(8) . ?
N5 C19 1.343(8) . ?
N5 C23 1.360(9) . ?
N6 N7 1.278(8) . ?
N6 C23 1.408(9) . ?
N7 C24 1.427(8) . ?
N8 C27 1.364(9) . ?
N8 C30 1.436(9) . ?
C1 C2 1.470(10) . ?
C2 C7 1.389(10) . ?
C2 C3 1.418(10) . ?
C3 C4 1.376(10) . ?
C4 C5 1.386(9) . ?
C5 C6 1.405(9) . ?
C6 C7 1.391(9) . ?
C8 C13 1.421(9) . ?
C8 C9 1.438(9) . ?
C9 C10 1.340(10) . ?
C10 C11 1.443(10) . ?
C11 C12 1.356(9) . ?
C12 C13 1.427(9) . ?
C14 C15 1.398(9) . ?
C15 C16 1.376(10) . ?
C16 C17 1.401(11) . ?
C17 C18 1.374(9) . ?
C19 C20 1.358(10) . ?
C20 C21 1.349(10) . ?
C21 C22 1.398(10) . ?
C22 C23 1.365(10) . ?
C24 C25 1.361(9) . ?
C24 C29 1.444(9) . ?
C25 C26 1.386(9) . ?
C26 C27 1.405(9) . ?
C27 C28 1.376(10) . ?
C28 C29 1.372(10) . ?
C30 C35 1.373(10) . ?
C30 C31 1.410(11) . ?
C31 C32 1.366(11) . ?
C32 C33 1.374(11) . ?
C33 C34 1.358(11) . ?
C33 C36 1.524(10) . ?
C34 C35 1.383(10) . ?
F1 P1 1.584(6) . ?
F2 P1 1.592(5) . ?
F3 P1 1.601(5) . ?
F4 P1 1.590(5) . ?
F5 P1 1.574(5) . ?
F6 P1 1.569(5) . ?
