#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/75/7027546.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_7027546
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 H27 Cl3 N4 O3.5 Rh'
_chemical_formula_weight         516.66
_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                67.21(3)
_cell_angle_beta                 94.35(3)
_cell_angle_gamma                82.12(3)
_cell_formula_units_Z            2
_cell_length_a                   8.524(2)
_cell_length_b                   11.529(2)
_cell_length_c                   12.116(2)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1076.5(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 0.815
_diffrn_measured_fraction_theta_max 0.815
_diffrn_measurement_device_type  'Syntex P-1'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0147
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3103
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.188
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             526
_exptl_crystal_size_max          .52
_exptl_crystal_size_mid          .50
_exptl_crystal_size_min          .10
_refine_diff_density_max         0.969
_refine_diff_density_min         -1.325
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0108(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refined
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.750
_refine_ls_shift/su_mean         0.073
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0608P)²+0.9751P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0824
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                3094
_reflns_number_total             3103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903844bsup1.cif
_cod_data_source_block           pmb21
_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^)+(0.0608P)^2^+0.9751P] 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^)+(0.0608P)^2^+0.9751P] 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        1076.5(4)
_cod_original_formula_sum        'C14 H27 Cl3 N4 O3.50 Rh'
_cod_database_code               7027546
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
Rh1 Rh 0.0000 0.0000 0.5000 0.02750(14) Uani 1 d S
Rh2 Rh 0.0000 0.0000 0.0000 0.02918(14) Uani 1 d S
Cl1 Cl 0.10725(11) 0.11850(9) 0.59583(9) 0.0434(2) Uani 1 d .
Cl2 Cl -0.19164(11) 0.04454(9) -0.16550(8) 0.0448(2) Uani 1 d .
Cl3 Cl -0.22255(14) 0.36506(10) 0.10285(10) 0.0586(3) Uani 1 d .
O1 O 0.2736(3) 0.0604(2) 0.3756(2) 0.0348(5) Uani 1 d .
N1 N 0.2199(3) -0.0472(3) 0.4629(2) 0.0305(6) Uani 1 d .
N2 N 0.0090(4) 0.1437(3) 0.3385(3) 0.0330(6) Uani 1 d .
C1 C 0.3219(4) -0.1496(3) 0.4904(3) 0.0323(7) Uani 1 d .
C2 C 0.4749(4) -0.1618(4) 0.4396(4) 0.0409(8) Uani 1 d .
C3 C 0.5514(6) -0.3015(4) 0.5109(5) 0.0626(13) Uani 1 d .
C4 C 0.4134(6) -0.3703(4) 0.5474(5) 0.0615(12) Uani 1 d .
C5 C 0.2963(5) -0.2769(4) 0.5762(4) 0.0468(9) Uani 1 d .
C6 C 0.1940(6) 0.2497(4) 0.1996(4) 0.0475(10) Uani 1 d .
C7 C 0.1467(4) 0.1514(3) 0.3062(3) 0.0343(7) Uani 1 d .
O1' O -0.2704(3) -0.0799(3) 0.1189(3) 0.0469(6) Uani 1 d .
N1' N -0.1157(4) -0.1347(3) 0.1018(3) 0.0375(7) Uani 1 d .
N2' N -0.1618(4) 0.0989(3) 0.0596(3) 0.0359(7) Uani 1 d .
C1' C -0.0837(5) -0.2542(4) 0.1661(3) 0.0445(9) Uani 1 d .
C2' C -0.1839(8) -0.3314(5) 0.2532(5) 0.0645(13) Uani 1 d .
C3' C -0.0813(10) -0.4635(6) 0.3112(7) 0.097(2) Uani 1 d .
C4' C 0.0840(11) -0.4480(6) 0.2912(7) 0.095(2) Uani 1 d .
C5' C 0.0712(7) -0.3355(4) 0.1699(5) 0.0580(11) Uani 1 d .
C6' C -0.4203(6) 0.0958(6) 0.1407(6) 0.0609(13) Uani 1 d .
C7' C -0.2745(4) 0.0428(4) 0.1039(3) 0.0401(8) Uani 1 d .
O1W O -0.4518(8) 0.4957(9) -0.1539(5) 0.179(4) Uani 1 d .
O2W O -0.444(3) 0.300(2) -0.219(3) 0.300(12) Uani 0.50 d P
H21 H 0.454(5) -0.142(4) 0.351(4) 0.041(10) Uiso 1 d .
H22 H 0.544(5) -0.108(4) 0.447(3) 0.037(10) Uiso 1 d .
H31 H 0.617(6) -0.327(4) 0.459(4) 0.063(13) Uiso 1 d .
H32 H 0.626(8) -0.318(6) 0.598(6) 0.10(2) Uiso 1 d .
H41 H 0.450(6) -0.462(5) 0.625(5) 0.071(15) Uiso 1 d .
H42 H 0.360(6) -0.375(5) 0.473(5) 0.072(16) Uiso 1 d .
H51 H 0.346(5) -0.285(4) 0.661(4) 0.051(12) Uiso 1 d .
H52 H 0.201(5) -0.288(4) 0.568(4) 0.048(12) Uiso 1 d .
H61 H 0.117(6) 0.310(5) 0.166(5) 0.069(16) Uiso 1 d .
H62 H 0.283(7) 0.281(5) 0.225(5) 0.076(16) Uiso 1 d .
H63 H 0.235(7) 0.209(6) 0.156(6) 0.10(2) Uiso 1 d .
H1N2 H -0.063(4) 0.196(4) 0.288(3) 0.029(9) Uiso 1 d .
H21' H -0.279(6) -0.325(5) 0.208(5) 0.070(16) Uiso 1 d .
H22' H -0.198(6) -0.300(5) 0.313(5) 0.069(15) Uiso 1 d .
H31' H -0.104(7) -0.493(6) 0.385(6) 0.087(19) Uiso 1 d .
H32' H -0.045(16) -0.500(11) 0.240(11) 0.23(5) Uiso 1 d .
H41' H 0.159(9) -0.513(7) 0.307(6) 0.11(2) Uiso 1 d .
H42' H 0.165(13) -0.433(11) 0.368(10) 0.20(5) Uiso 1 d .
H51' H 0.155(6) -0.299(5) 0.172(4) 0.055(14) Uiso 1 d .
H52' H 0.061(6) -0.353(5) 0.097(5) 0.075(15) Uiso 1 d .
H61' H -0.402(7) 0.063(6) 0.227(6) 0.10(2) Uiso 1 d .
H62' H -0.417(7) 0.177(7) 0.129(6) 0.10(2) Uiso 1 d .
H63' H -0.500(8) 0.079(7) 0.112(6) 0.10(2) Uiso 1 d .
H2N' H -0.164(5) 0.167(4) 0.053(3) 0.033(11) Uiso 1 d .
H1W1 H -0.525(4) 0.406(3) -0.097(3) 0.016(8) Uiso 1 d .
H2W1 H -0.375(16) 0.489(14) -0.046(13) 0.34(7) 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'
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'
O O 0.0106 0.0060 '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
N1 Rh1 N1 180.0 . 2_556
N1 Rh1 N2 103.38(12) . 2_556
N1 Rh1 N2 76.62(12) 2_556 2_556
N1 Rh1 N2 76.62(12) . .
N1 Rh1 N2 103.38(12) 2_556 .
N2 Rh1 N2 180.0 2_556 .
N1 Rh1 Cl1 91.40(9) . 2_556
N1 Rh1 Cl1 88.60(9) 2_556 2_556
N2 Rh1 Cl1 88.53(9) 2_556 2_556
N2 Rh1 Cl1 91.47(9) . 2_556
N1 Rh1 Cl1 88.60(9) . .
N1 Rh1 Cl1 91.40(9) 2_556 .
N2 Rh1 Cl1 91.47(9) 2_556 .
N2 Rh1 Cl1 88.53(9) . .
Cl1 Rh1 Cl1 180.0 2_556 .
N1' Rh2 N1' 180.0 2 .
N1' Rh2 N2' 76.97(13) 2 2
N1' Rh2 N2' 103.03(13) . 2
N1' Rh2 N2' 103.03(13) 2 .
N1' Rh2 N2' 76.97(13) . .
N2' Rh2 N2' 180.0 2 .
N1' Rh2 Cl2 89.10(10) 2 2
N1' Rh2 Cl2 90.90(10) . 2
N2' Rh2 Cl2 87.85(10) 2 2
N2' Rh2 Cl2 92.15(10) . 2
N1' Rh2 Cl2 90.90(10) 2 .
N1' Rh2 Cl2 89.10(10) . .
N2' Rh2 Cl2 92.15(10) 2 .
N2' Rh2 Cl2 87.85(10) . .
Cl2 Rh2 Cl2 180.0 2 .
C7 O1 N1 110.5(3) . .
C1 N1 O1 110.4(3) . .
C1 N1 Rh1 136.8(3) . .
O1 N1 Rh1 112.61(19) . .
C7 N2 Rh1 115.9(3) . .
N1 C1 C5 122.5(3) . .
N1 C1 C2 126.6(3) . .
C5 C1 C2 110.9(3) . .
C1 C2 C3 103.4(3) . .
C4 C3 C2 105.1(4) . .
C3 C4 C5 103.9(4) . .
C1 C5 C4 103.0(4) . .
N2 C7 O1 119.1(3) . .
N2 C7 C6 128.9(4) . .
O1 C7 C6 112.0(3) . .
C7' O1' N1' 110.9(3) . .
C1' N1' O1' 110.5(3) . .
C1' N1' Rh2 137.0(3) . .
O1' N1' Rh2 111.9(2) . .
C7' N2' Rh2 115.7(3) . .
N1' C1' C2' 126.7(4) . .
N1' C1' C5' 122.4(4) . .
C2' C1' C5' 110.7(4) . .
C1' C2' C3' 103.6(5) . .
C4' C3' C2' 107.0(5) . .
C3' C4' C5' 105.9(7) . .
C1' C5' C4' 102.0(5) . .
N2' C7' O1' 119.2(3) . .
N2' C7' C6' 128.3(4) . .
O1' C7' C6' 112.6(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 2.013(3) .
Rh1 N1 2.013(3) 2_556
Rh1 N2 2.031(3) 2_556
Rh1 N2 2.031(3) .
Rh1 Cl1 2.3368(11) 2_556
Rh1 Cl1 2.3368(11) .
Rh2 N1' 2.007(3) 2
Rh2 N1' 2.007(3) .
Rh2 N2' 2.020(3) 2
Rh2 N2' 2.020(3) .
Rh2 Cl2 2.3299(13) 2
Rh2 Cl2 2.3299(13) .
O1 C7 1.358(5) .
O1 N1 1.442(4) .
N1 C1 1.276(5) .
N2 C7 1.269(5) .
C1 C5 1.491(6) .
C1 C2 1.497(5) .
C2 C3 1.521(6) .
C3 C4 1.507(8) .
C4 C5 1.525(6) .
C6 C7 1.479(6) .
O1' C7' 1.349(5) .
O1' N1' 1.447(4) .
N1' C1' 1.269(5) .
N2' C7' 1.268(5) .
C1' C2' 1.501(6) .
C1' C5' 1.497(7) .
C2' C3' 1.513(10) .
C3' C4' 1.471(12) .
C4' C5' 1.521(8) .
C6' C7' 1.484(6) .
