#------------------------------------------------------------------------------
#$Date: 2016-03-25 08:53:21 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179710 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/13/7001348.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_7001348
loop_
_publ_author_name
'Hounjet, Lindsay J.'
'Bierenstiel, Matthias'
'Ferguson, Michael J.'
'McDonald, Robert'
'Cowie, Martin'
_publ_section_title
;
 Mono- and binuclear complexes of rhodium involving a new series of
 hemilabile o-phosphinoaniline ligands
;
_journal_issue                   21
_journal_name_full               'Dalton Transactions'
_journal_page_first              4213
_journal_page_last               4226
_journal_paper_doi               10.1039/b822170g
_journal_year                    2009
_chemical_formula_moiety         'C22 H24 Cl N3 O P Rh'
_chemical_formula_sum            'C22 H24 Cl N3 O P Rh'
_chemical_formula_weight         515.77
_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                85.0063(12)
_cell_angle_beta                 77.9072(12)
_cell_angle_gamma                72.8739(11)
_cell_formula_units_Z            2
_cell_length_a                   9.3726(8)
_cell_length_b                   11.3968(10)
_cell_length_c                   11.4388(10)
_cell_measurement_reflns_used    5134
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.32
_cell_volume                     1141.36(17)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       'ω 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  0.0119
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10067
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.953
_exptl_absorpt_correction_T_max  0.7898
_exptl_absorpt_correction_T_min  0.6848
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         5172
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0216
_refine_ls_R_factor_gt           0.0206
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0327P)²+0.3460P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                4964
_reflns_number_total             5172
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b822170g.txt
_cod_data_source_block           compound(7)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7001348
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
Rh Rh 0.218969(12) 0.099411(9) 0.311255(9) 0.02336(5) Uani 1 1 d . . .
Cl Cl 0.22942(5) -0.08655(4) 0.42549(4) 0.03919(10) Uani 1 1 d . . .
P P 0.18144(4) 0.26610(3) 0.19276(3) 0.02262(8) Uani 1 1 d . . .
O O 0.53144(16) 0.09286(15) 0.32820(18) 0.0625(4) Uani 1 1 d . . .
N1 N -0.01518(14) 0.11800(12) 0.31343(12) 0.0280(3) Uani 1 1 d . . .
H1N H -0.0581 0.1027 0.3921 0.034 Uiso 1 1 calc R . .
N2 N 0.50875(17) 0.18390(15) 0.04350(14) 0.0425(3) Uani 1 1 d . . .
H2N H 0.4834 0.2189 0.1133 0.051 Uiso 1 1 calc R . .
N3 N 0.16847(18) 0.37321(14) 0.43168(12) 0.0371(3) Uani 1 1 d . . .
H3N H 0.1291 0.3148 0.4206 0.044 Uiso 1 1 calc R . .
C1 C 0.4121(2) 0.09443(15) 0.31940(17) 0.0363(4) Uani 1 1 d . . .
C11 C -0.02507(17) 0.32143(13) 0.21866(13) 0.0253(3) Uani 1 1 d . . .
C12 C -0.10300(17) 0.24147(14) 0.28091(13) 0.0270(3) Uani 1 1 d . . .
C13 C -0.26087(19) 0.27761(17) 0.31050(17) 0.0375(4) Uani 1 1 d . . .
H13 H -0.3137 0.2233 0.3544 0.045 Uiso 1 1 calc R . .
C14 C -0.34075(19) 0.39375(18) 0.27538(18) 0.0415(4) Uani 1 1 d . . .
H14 H -0.4488 0.4186 0.2946 0.050 Uiso 1 1 calc R . .
C15 C -0.2641(2) 0.47418(16) 0.21226(16) 0.0364(4) Uani 1 1 d . . .
H15 H -0.3196 0.5534 0.1882 0.044 Uiso 1 1 calc R . .
C16 C -0.10687(19) 0.43856(14) 0.18455(14) 0.0310(3) Uani 1 1 d . . .
H16 H -0.0543 0.4938 0.1422 0.037 Uiso 1 1 calc R . .
C17 C -0.0349(2) 0.02350(17) 0.2406(2) 0.0446(4) Uani 1 1 d . . .
H17A H 0.0248 -0.0581 0.2636 0.053 Uiso 1 1 calc R . .
H17B H 0.0002 0.0402 0.1556 0.053 Uiso 1 1 calc R . .
H17C H -0.1427 0.0264 0.2547 0.053 Uiso 1 1 calc R . .
C21 C 0.24048(19) 0.23863(13) 0.03292(13) 0.0287(3) Uani 1 1 d . . .
C22 C 0.3971(2) 0.19516(14) -0.02082(15) 0.0338(3) Uani 1 1 d . . .
C23 C 0.4336(2) 0.16478(16) -0.14237(16) 0.0438(4) Uani 1 1 d . . .
H23 H 0.5374 0.1350 -0.1801 0.053 Uiso 1 1 calc R . .
C24 C 0.3219(3) 0.17738(17) -0.20731(16) 0.0492(5) Uani 1 1 d . . .
H24 H 0.3499 0.1568 -0.2893 0.059 Uiso 1 1 calc R . .
C25 C 0.1695(3) 0.21948(17) -0.15559(16) 0.0451(4) Uani 1 1 d . . .
H25 H 0.0932 0.2277 -0.2013 0.054 Uiso 1 1 calc R . .
C26 C 0.1300(2) 0.24951(15) -0.03564(14) 0.0346(3) Uani 1 1 d . . .
H26 H 0.0255 0.2781 0.0005 0.041 Uiso 1 1 calc R . .
C27 C 0.6671(2) 0.11668(19) 0.0016(2) 0.0517(5) Uani 1 1 d . . .
H27A H 0.6733 0.0335 -0.0194 0.062 Uiso 1 1 calc R . .
H27B H 0.7248 0.1120 0.0649 0.062 Uiso 1 1 calc R . .
H27C H 0.7099 0.1593 -0.0691 0.062 Uiso 1 1 calc R . .
C31 C 0.23699(17) 0.40036(13) 0.21693(13) 0.0255(3) Uani 1 1 d . . .
C32 C 0.21933(17) 0.43943(14) 0.33494(14) 0.0291(3) Uani 1 1 d . . .
C33 C 0.2489(2) 0.55127(16) 0.34831(17) 0.0385(4) Uani 1 1 d . . .
H33 H 0.2352 0.5806 0.4263 0.046 Uiso 1 1 calc R . .
C34 C 0.2974(2) 0.61896(16) 0.2504(2) 0.0446(4) Uani 1 1 d . . .
H34 H 0.3153 0.6946 0.2619 0.054 Uiso 1 1 calc R . .
C35 C 0.3204(2) 0.57835(16) 0.13609(19) 0.0441(4) Uani 1 1 d . . .
H35 H 0.3575 0.6240 0.0692 0.053 Uiso 1 1 calc R . .
C36 C 0.2889(2) 0.46997(15) 0.11961(15) 0.0343(3) Uani 1 1 d . . .
H36 H 0.3029 0.4427 0.0408 0.041 Uiso 1 1 calc R . .
C37 C 0.1775(3) 0.3966(2) 0.55215(17) 0.0532(5) Uani 1 1 d . . .
H37A H 0.2830 0.3908 0.5555 0.064 Uiso 1 1 calc R . .
H37B H 0.1432 0.3356 0.6079 0.064 Uiso 1 1 calc R . .
H37C H 0.1125 0.4791 0.5745 0.064 Uiso 1 1 calc R . .
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'
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
C1 Rh N1 174.80(6) . . ?
C1 Rh P 95.00(6) . . ?
N1 Rh P 84.05(4) . . ?
C1 Rh Cl 93.16(5) . . ?
N1 Rh Cl 88.16(4) . . ?
P Rh Cl 171.011(16) . . ?
C31 P C11 103.35(7) . . ?
C31 P C21 106.04(7) . . ?
C11 P C21 105.07(7) . . ?
C31 P Rh 122.75(5) . . ?
C11 P Rh 101.89(5) . . ?
C21 P Rh 115.52(5) . . ?
C12 N1 C17 110.83(13) . . ?
C12 N1 Rh 114.46(9) . . ?
C17 N1 Rh 112.21(10) . . ?
C22 N2 C27 122.99(17) . . ?
C32 N3 C37 121.80(17) . . ?
O C1 Rh 177.73(19) . . ?
C12 C11 C16 119.50(14) . . ?
C12 C11 P 116.19(11) . . ?
C16 C11 P 124.26(12) . . ?
C13 C12 C11 120.54(14) . . ?
C13 C12 N1 120.82(14) . . ?
C11 C12 N1 118.63(13) . . ?
C14 C13 C12 119.40(16) . . ?
C13 C14 C15 120.58(16) . . ?
C16 C15 C14 119.86(15) . . ?
C15 C16 C11 120.12(15) . . ?
C26 C21 C22 119.38(15) . . ?
C26 C21 P 119.30(12) . . ?
C22 C21 P 121.04(13) . . ?
N2 C22 C23 121.15(17) . . ?
N2 C22 C21 121.03(15) . . ?
C23 C22 C21 117.81(17) . . ?
C24 C23 C22 121.22(18) . . ?
C23 C24 C25 121.24(17) . . ?
C24 C25 C26 118.83(19) . . ?
C25 C26 C21 121.50(18) . . ?
C36 C31 C32 119.56(14) . . ?
C36 C31 P 120.27(12) . . ?
C32 C31 P 120.06(11) . . ?
N3 C32 C33 121.43(15) . . ?
N3 C32 C31 120.75(14) . . ?
C33 C32 C31 117.75(15) . . ?
C34 C33 C32 121.25(16) . . ?
C35 C34 C33 120.88(16) . . ?
C34 C35 C36 119.32(17) . . ?
C35 C36 C31 121.15(16) . . ?
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
Rh C1 1.8160(17) . ?
Rh N1 2.1368(13) . ?
Rh P 2.2199(4) . ?
Rh Cl 2.3787(4) . ?
P C31 1.8143(15) . ?
P C11 1.8180(15) . ?
P C21 1.8223(15) . ?
O C1 1.139(2) . ?
N1 C12 1.4666(19) . ?
N1 C17 1.492(2) . ?
N2 C22 1.371(2) . ?
N2 C27 1.455(2) . ?
N3 C32 1.366(2) . ?
N3 C37 1.450(2) . ?
C11 C12 1.390(2) . ?
C11 C16 1.398(2) . ?
C12 C13 1.389(2) . ?
C13 C14 1.387(2) . ?
C14 C15 1.390(3) . ?
C15 C16 1.382(2) . ?
C21 C26 1.396(2) . ?
C21 C22 1.423(2) . ?
C22 C23 1.409(2) . ?
C23 C24 1.374(3) . ?
C24 C25 1.383(3) . ?
C25 C26 1.390(2) . ?
C31 C36 1.397(2) . ?
C31 C32 1.420(2) . ?
C32 C33 1.409(2) . ?
C33 C34 1.378(3) . ?
C34 C35 1.378(3) . ?
C35 C36 1.388(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N Cl 0.93 2.38 3.2870(14) 164.7 2_556
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 Rh P C31 -44.49(8) . . . . ?
N1 Rh P C31 130.38(7) . . . . ?
Cl Rh P C31 160.42(10) . . . . ?
C1 Rh P C11 -159.07(8) . . . . ?
N1 Rh P C11 15.80(6) . . . . ?
Cl Rh P C11 45.84(11) . . . . ?
C1 Rh P C21 87.67(8) . . . . ?
N1 Rh P C21 -97.47(7) . . . . ?
Cl Rh P C21 -67.42(11) . . . . ?
C1 Rh N1 C12 58.9(7) . . . . ?
P Rh N1 C12 -20.84(10) . . . . ?
Cl Rh N1 C12 163.64(10) . . . . ?
C1 Rh N1 C17 -173.7(7) . . . . ?
P Rh N1 C17 106.57(11) . . . . ?
Cl Rh N1 C17 -68.94(11) . . . . ?
N1 Rh C1 O 24(5) . . . . ?
P Rh C1 O 103(4) . . . . ?
Cl Rh C1 O -81(4) . . . . ?
C31 P C11 C12 -139.78(12) . . . . ?
C21 P C11 C12 109.24(12) . . . . ?
Rh P C11 C12 -11.61(12) . . . . ?
C31 P C11 C16 37.53(15) . . . . ?
C21 P C11 C16 -73.45(14) . . . . ?
Rh P C11 C16 165.71(12) . . . . ?
C16 C11 C12 C13 -0.8(2) . . . . ?
P C11 C12 C13 176.69(13) . . . . ?
C16 C11 C12 N1 178.60(14) . . . . ?
P C11 C12 N1 -3.95(19) . . . . ?
C17 N1 C12 C13 70.5(2) . . . . ?
Rh N1 C12 C13 -161.39(13) . . . . ?
C17 N1 C12 C11 -108.87(16) . . . . ?
Rh N1 C12 C11 19.26(17) . . . . ?
C11 C12 C13 C14 1.2(3) . . . . ?
N1 C12 C13 C14 -178.12(16) . . . . ?
C12 C13 C14 C15 -0.7(3) . . . . ?
C13 C14 C15 C16 -0.3(3) . . . . ?
C14 C15 C16 C11 0.7(3) . . . . ?
C12 C11 C16 C15 -0.2(2) . . . . ?
P C11 C16 C15 -177.46(13) . . . . ?
C31 P C21 C26 -115.61(12) . . . . ?
C11 P C21 C26 -6.57(14) . . . . ?
Rh P C21 C26 104.84(12) . . . . ?
C31 P C21 C22 70.38(13) . . . . ?
C11 P C21 C22 179.42(12) . . . . ?
Rh P C21 C22 -69.17(13) . . . . ?
C27 N2 C22 C23 -13.7(3) . . . . ?
C27 N2 C22 C21 166.65(16) . . . . ?
C26 C21 C22 N2 179.64(15) . . . . ?
P C21 C22 N2 -6.4(2) . . . . ?
C26 C21 C22 C23 0.0(2) . . . . ?
P C21 C22 C23 174.00(12) . . . . ?
N2 C22 C23 C24 -179.22(17) . . . . ?
C21 C22 C23 C24 0.4(2) . . . . ?
C22 C23 C24 C25 -0.5(3) . . . . ?
C23 C24 C25 C26 0.1(3) . . . . ?
C24 C25 C26 C21 0.3(3) . . . . ?
C22 C21 C26 C25 -0.4(2) . . . . ?
P C21 C26 C25 -174.47(13) . . . . ?
C11 P C31 C36 -100.71(13) . . . . ?
C21 P C31 C36 9.56(15) . . . . ?
Rh P C31 C36 145.44(11) . . . . ?
C11 P C31 C32 75.53(13) . . . . ?
C21 P C31 C32 -174.20(12) . . . . ?
Rh P C31 C32 -38.32(14) . . . . ?
C37 N3 C32 C33 -15.4(2) . . . . ?
C37 N3 C32 C31 167.65(16) . . . . ?
C36 C31 C32 N3 179.86(15) . . . . ?
P C31 C32 N3 3.6(2) . . . . ?
C36 C31 C32 C33 2.8(2) . . . . ?
P C31 C32 C33 -173.42(12) . . . . ?
N3 C32 C33 C34 -178.75(16) . . . . ?
C31 C32 C33 C34 -1.8(2) . . . . ?
C32 C33 C34 C35 -0.9(3) . . . . ?
C33 C34 C35 C36 2.3(3) . . . . ?
C34 C35 C36 C31 -1.2(3) . . . . ?
C32 C31 C36 C35 -1.4(2) . . . . ?
P C31 C36 C35 174.82(14) . . . . ?
