#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027547.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7027547
loop_
_publ_author_name
'Yu. Kukushkin, Vadim'
'Ilichev, Igor V.'
'Wagner, Gabriele'
'Fraústo da Silva, João J. R.'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Rhodium(III)-mediated oxime--nitrile coupling giving chelated
 iminoacylated species †
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3047
_journal_paper_doi               10.1039/a903844b
_journal_year                    1999
_chemical_formula_sum            'C14 H21 Cl1.5 N2 O2.5 Rh0.5'
_chemical_formula_weight         361.96
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.58(3)
_cell_angle_beta                 97.65(3)
_cell_angle_gamma                112.09(3)
_cell_formula_units_Z            2
_cell_length_a                   8.866(2)
_cell_length_b                   10.358(2)
_cell_length_c                   10.952(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10
_cell_volume                     838.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.550
_diffrn_measured_fraction_theta_max 0.550
_diffrn_measurement_device_type  CAD-4
_diffrn_measurement_method       theta/2theta
_diffrn_radiation_monochromator  beta-filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1751
_diffrn_reflns_theta_full        24.96
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        5
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.789
_exptl_absorpt_correction_T_max  0.965
_exptl_absorpt_correction_T_min  0.846
_exptl_absorpt_correction_type   numeric
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.690
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0775P)²+0.2425P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                1618
_reflns_number_total             1618
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903844bsup1.cif
_cod_data_source_block           vk06
_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 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+0.2425P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0775P)^2^+0.2425P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        838.5(3)
_cod_original_formula_sum        'C14 H21 Cl1.50 N2 O2.50 Rh0.50'
_cod_database_code               7027547
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_calc_flag
_atom_site_refinement_flags
Rh Rh 0.5000 0.5000 0.5000 0.0385(2) Uani 1 d S
Cl1 Cl 0.21684(17) 0.41480(13) 0.38275(14) 0.0536(4) Uani 1 d .
O1 O 0.3990(5) 0.1818(3) 0.3349(4) 0.0514(9) Uani 1 d .
N1 N 0.4224(6) 0.3215(4) 0.5515(5) 0.0436(10) Uani 1 d .
N2 N 0.5084(5) 0.3327(4) 0.3460(4) 0.0445(10) Uani 1 d .
C1 C 0.3765(6) 0.1903(5) 0.4562(5) 0.0433(12) Uani 1 d .
C2 C 0.2972(7) 0.0398(5) 0.4600(6) 0.0477(13) Uani 1 d .
C3 C 0.3130(7) -0.0839(5) 0.3733(7) 0.0544(14) Uani 1 d .
C4 C 0.2396(8) -0.2232(7) 0.3823(8) 0.0647(17) Uani 1 d .
C5 C 0.1546(9) -0.2387(7) 0.4763(8) 0.0729(19) Uani 1 d .
C6 C 0.1347(9) -0.1177(7) 0.5595(8) 0.0721(19) Uani 1 d .
C7 C 0.2079(8) 0.0233(7) 0.5528(7) 0.0613(16) Uani 1 d .
C8 C 0.5921(7) 0.3220(6) 0.2593(5) 0.0497(13) Uani 1 d .
C9 C 0.5851(11) 0.1774(7) 0.1614(8) 0.0671(18) Uani 1 d .
C10 C 0.7105(13) 0.2292(9) 0.0868(10) 0.103(3) Uani 1 d .
C11 C 0.8233(10) 0.3954(9) 0.1709(10) 0.084(2) Uani 1 d .
C12 C 0.7189(9) 0.4589(7) 0.2484(8) 0.0596(16) Uani 1 d .
Cl2 Cl 0.5215(14) 0.3328(14) -0.1596(9) 0.0851(18) Uani 0.50 d P
O1W O 0.507(5) 0.364(4) -0.165(3) 0.125(12) Uani 0.50 d P
O1E O 0.3242(16) 0.3262(13) 0.0168(11) 0.188(4) Uiso 1 d .
C1E C 0.144(3) 0.215(2) -0.007(2) 0.213(7) Uiso 1 d .
C2EA C 0.050(3) 0.217(3) -0.100(3) 0.137(8) Uiso 0.50 d P
C2EB C 0.050(3) 0.112(3) -0.125(3) 0.137(8) Uiso 0.50 d P
H1N H 0.424(6) 0.319(5) 0.632(6) 0.038(14) Uiso 1 d .
H3 H 0.372(7) -0.066(5) 0.305(5) 0.040(13) Uiso 1 d .
H4 H 0.252(9) -0.299(8) 0.328(7) 0.07(2) Uiso 1 d .
H5 H 0.101(8) -0.333(7) 0.492(6) 0.062(16) Uiso 1 d .
H6 H 0.079(9) -0.140(8) 0.625(7) 0.09(2) Uiso 1 d .
H7 H 0.189(7) 0.100(6) 0.611(5) 0.047(15) Uiso 1 d .
H91 H 0.460(12) 0.102(10) 0.123(8) 0.11(3) Uiso 1 d .
H92 H 0.583(9) 0.127(7) 0.202(7) 0.06(2) Uiso 1 d .
H101 H 0.755(9) 0.153(8) 0.042(7) 0.09(2) Uiso 1 d .
H102 H 0.625(18) 0.260(15) -0.017(14) 0.23(6) Uiso 1 d .
H111 H 0.890(9) 0.450(8) 0.139(7) 0.07(2) Uiso 1 d .
H112 H 0.884(16) 0.392(13) 0.277(13) 0.19(5) Uiso 1 d .
H121 H 0.775(7) 0.551(7) 0.330(6) 0.048(14) Uiso 1 d .
H122 H 0.660(10) 0.480(8) 0.205(8) 0.08(3) Uiso 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'
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
N2 Rh N2 180.0 2_666 .
N2 Rh N1 103.25(17) 2_666 .
N2 Rh N1 76.75(17) . .
N2 Rh N1 76.75(17) 2_666 2_666
N2 Rh N1 103.25(17) . 2_666
N1 Rh N1 180.0 . 2_666
N2 Rh Cl1 88.75(14) 2_666 2_666
N2 Rh Cl1 91.25(14) . 2_666
N1 Rh Cl1 91.26(13) . 2_666
N1 Rh Cl1 88.74(13) 2_666 2_666
N2 Rh Cl1 91.25(14) 2_666 .
N2 Rh Cl1 88.75(14) . .
N1 Rh Cl1 88.74(13) . .
N1 Rh Cl1 91.26(13) 2_666 .
Cl1 Rh Cl1 180.0 2_666 .
C1 O1 N2 110.3(3) . .
C1 N1 Rh 115.8(4) . .
C8 N2 O1 110.4(4) . .
C8 N2 Rh 137.5(3) . .
O1 N2 Rh 111.8(3) . .
N1 C1 O1 119.0(4) . .
N1 C1 C2 127.6(5) . .
O1 C1 C2 113.4(4) . .
C3 C2 C7 120.3(5) . .
C3 C2 C1 120.6(5) . .
C7 C2 C1 119.1(5) . .
C2 C3 C4 118.8(6) . .
C5 C4 C3 121.0(6) . .
C6 C5 C4 120.3(6) . .
C5 C6 C7 119.7(7) . .
C2 C7 C6 119.9(6) . .
N2 C8 C9 126.3(5) . .
N2 C8 C12 122.9(5) . .
C9 C8 C12 110.7(5) . .
C8 C9 C10 104.8(6) . .
C11 C10 C9 106.6(7) . .
C10 C11 C12 106.7(6) . .
C8 C12 C11 103.0(5) . .
C2EA C1E C2EB 48.6(16) . .
C2EA C1E O1E 109(2) . .
C2EB C1E O1E 121(2) . .
C2EB C2EA C1E 68(2) . .
C2EA C2EB C1E 64(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh N2 2.006(4) 2_666
Rh N2 2.006(4) .
Rh N1 2.014(4) .
Rh N1 2.014(4) 2_666
Rh Cl1 2.3337(17) 2_666
Rh Cl1 2.3337(17) .
O1 C1 1.349(6) .
O1 N2 1.449(5) .
N1 C1 1.274(6) .
N2 C8 1.282(7) .
C1 C2 1.467(6) .
C2 C3 1.384(8) .
C2 C7 1.384(8) .
C3 C4 1.386(7) .
C4 C5 1.371(10) .
C5 C6 1.370(10) .
C6 C7 1.390(8) .
C8 C9 1.494(8) .
C8 C12 1.496(8) .
C9 C10 1.509(11) .
C10 C11 1.487(10) .
C11 C12 1.518(10) .
O1E C1E 1.50(2) .
C1E C2EA 1.24(3) .
C1E C2EB 1.28(3) .
C2EA C2EB 1.04(3) .
