#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:38:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179981 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027545.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_7027545
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            'C12 H21 Cl3 N3 O2 Rh'
_chemical_formula_weight         448.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.512(2)
_cell_length_b                   9.724(2)
_cell_length_c                   15.694(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      11.3
_cell_volume                     1679.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.631
_diffrn_measured_fraction_theta_max 0.631
_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  0.0138
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2090
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        .2
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.500
_exptl_absorpt_correction_T_max  0.8645
_exptl_absorpt_correction_T_min  0.3454
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         1982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0371P)²+0.9685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0559
_reflns_number_gt                1982
_reflns_number_total             1982
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903844bsup1.cif
_cod_data_source_block           pmb19
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0371P)^2^+0.9685P] 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^)+(0.0371P)^2^+0.9685P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7027545
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
Rh Rh 0.30474(2) 0.10028(2) 0.724883(16) 0.03143(10) Uani 1 d
Cl1 Cl 0.29430(9) -0.08414(9) 0.62954(6) 0.0481(2) Uani 1 d
Cl2 Cl 0.41131(8) 0.22984(9) 0.64741(6) 0.0419(2) Uani 1 d
Cl3 Cl 0.20678(10) -0.02406(10) 0.81239(7) 0.0543(3) Uani 1 d
O1 O 0.0523(3) 0.1841(3) 0.69819(19) 0.0617(8) Uani 1 d
O2 O 0.4464(2) 0.2146(2) 0.89312(15) 0.0415(6) Uani 1 d
N1 N 0.1369(3) 0.1695(3) 0.64830(18) 0.0364(6) Uani 1 d
N2 N 0.3439(2) 0.2521(3) 0.81729(17) 0.0357(6) Uani 1 d
N3 N 0.4608(3) 0.0352(3) 0.8060(2) 0.0395(7) Uani 1 d
C1 C 0.0891(3) 0.2088(4) 0.5694(2) 0.0461(9) Uani 1 d
C2 C -0.0366(4) 0.2648(5) 0.5326(3) 0.0562(11) Uani 1 d
C3 C -0.0408(5) 0.3111(6) 0.4387(3) 0.0692(13) Uani 1 d
C4 C 0.0436(5) 0.2121(6) 0.4128(3) 0.0703(13) Uani 1 d
C5 C 0.1515(4) 0.2021(6) 0.4976(3) 0.0607(11) Uani 1 d
C6 C 0.3159(3) 0.3776(3) 0.8260(2) 0.0352(7) Uani 1 d
C7 C 0.2185(4) 0.4518(4) 0.7572(3) 0.0446(9) Uani 1 d
C8 C 0.2473(5) 0.6028(4) 0.7832(3) 0.0550(10) Uani 1 d
C9 C 0.3013(5) 0.6005(4) 0.8817(3) 0.0549(11) Uani 1 d
C10 C 0.3781(4) 0.4704(4) 0.9015(3) 0.0403(8) Uani 1 d
C11 C 0.5045(3) 0.1018(3) 0.8773(2) 0.0387(8) Uani 1 d
C12 C 0.6179(5) 0.0754(5) 0.9498(3) 0.0525(11) Uani 1 d
H3N H 0.497(4) -0.033(4) 0.805(3) 0.050(12) Uiso 1 d
H21 H -0.057(4) 0.323(5) 0.569(3) 0.072(16) Uiso 1 d
H22 H -0.090(5) 0.183(6) 0.536(3) 0.086(16) Uiso 1 d
H31 H -0.007(6) 0.429(7) 0.450(4) 0.12(2) Uiso 1 d
H32 H -0.126(5) 0.313(5) 0.400(3) 0.079(15) Uiso 1 d
H41 H 0.076(5) 0.231(6) 0.364(4) 0.101(19) Uiso 1 d
H42 H -0.004(5) 0.102(6) 0.392(4) 0.092(17) Uiso 1 d
H51 H 0.196(5) 0.102(6) 0.504(4) 0.11(2) Uiso 1 d
H52 H 0.194(5) 0.307(6) 0.488(3) 0.088(16) Uiso 1 d
H71 H 0.144(4) 0.429(4) 0.764(3) 0.043(11) Uiso 1 d
H72 H 0.213(4) 0.430(5) 0.697(3) 0.064(14) Uiso 1 d
H81 H 0.175(4) 0.654(5) 0.768(3) 0.060(13) Uiso 1 d
H82 H 0.307(4) 0.637(5) 0.760(3) 0.063(14) Uiso 1 d
H91 H 0.232(4) 0.589(5) 0.912(3) 0.071(14) Uiso 1 d
H92 H 0.342(4) 0.674(5) 0.901(3) 0.060(13) Uiso 1 d
H101 H 0.451(4) 0.478(4) 0.896(2) 0.039(11) Uiso 1 d
H102 H 0.389(3) 0.427(4) 0.961(3) 0.041(10) Uiso 1 d
H121 H 0.636(5) -0.011(6) 0.943(3) 0.074(16) Uiso 1 d
H122 H 0.668(5) 0.128(6) 0.946(4) 0.09(2) Uiso 1 d
H123 H 0.601(4) 0.076(5) 1.000(4) 0.071(17) Uiso 1 d
H1O H 0.0720 0.1061 0.7491 0.050 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
N3 Rh N2 78.61(12)
N3 Rh N1 175.70(12)
N2 Rh N1 98.79(11)
N3 Rh Cl1 91.93(10)
N2 Rh Cl1 170.22(8)
N1 Rh Cl1 90.80(8)
N3 Rh Cl2 89.48(10)
N2 Rh Cl2 86.50(9)
N1 Rh Cl2 93.80(8)
Cl1 Rh Cl2 90.97(4)
N3 Rh Cl3 87.72(10)
N2 Rh Cl3 90.04(9)
N1 Rh Cl3 88.86(9)
Cl1 Rh Cl3 92.08(4)
Cl2 Rh Cl3 175.92(4)
C11 O2 N2 112.4(2)
C1 N1 O1 109.9(3)
C1 N1 Rh 137.3(3)
O1 N1 Rh 112.7(2)
C6 N2 O2 108.7(3)
C6 N2 Rh 139.6(2)
O2 N2 Rh 111.06(18)
C11 N3 Rh 117.2(3)
N1 C1 C2 125.7(4)
N1 C1 C5 123.9(4)
C2 C1 C5 110.4(4)
C1 C2 C3 103.4(4)
C4 C3 C2 103.4(4)
C3 C4 C5 103.2(4)
C1 C5 C4 101.7(4)
N2 C6 C10 125.7(3)
N2 C6 C7 122.9(3)
C10 C6 C7 111.4(3)
C6 C7 C8 102.2(3)
C9 C8 C7 104.7(4)
C8 C9 C10 105.3(3)
C6 C10 C9 103.1(3)
N3 C11 O2 119.4(3)
N3 C11 C12 128.6(4)
O2 C11 C12 111.9(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh N3 1.977(3)
Rh N2 2.025(3)
Rh N1 2.066(3)
Rh Cl1 2.3160(9)
Rh Cl2 2.3337(10)
Rh Cl3 2.3513(11)
O1 N1 1.424(4)
O2 C11 1.345(4)
O2 N2 1.456(3)
N1 C1 1.258(4)
N2 C6 1.280(4)
N3 C11 1.261(5)
C1 C2 1.495(6)
C1 C5 1.504(6)
C2 C3 1.529(6)
C3 C4 1.505(8)
C4 C5 1.535(6)
C6 C10 1.495(5)
C6 C7 1.494(5)
C7 C8 1.534(6)
C8 C9 1.488(6)
C9 C10 1.522(6)
C11 C12 1.481(5)
