#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:36:18 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179798 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/94/7009482.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_7009482
loop_
_publ_author_name
'Kukushkin, Vadim Yu.'
'Ilichev, Igor V.'
'Zhdanova, Maria A.'
'Wagner, Gabriele'
'Pombeiro, Armando J. L.'
_publ_section_title
;
 Metal-mediated hydrolysis of the oxime CN bond to produce
 RhIII-bound O-iminoacylated MeC(NH)ONH2 species
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1567
_journal_paper_doi               10.1039/b001384f
_journal_year                    2000
_chemical_formula_sum            'C4 H12 Cl3 N4 O2 Rh'
_chemical_formula_weight         357.44
_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                87.86(3)
_cell_angle_beta                 79.59(3)
_cell_angle_gamma                80.42(3)
_cell_formula_units_Z            2
_cell_length_a                   8.483(2)
_cell_length_b                   8.508(2)
_cell_length_c                   8.617(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      8.5
_cell_volume                     603.1(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.827
_diffrn_measured_fraction_theta_max 0.827
_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           AgK\a
_diffrn_radiation_wavelength     0.56083
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2027
_diffrn_reflns_theta_full        19.97
_diffrn_reflns_theta_max         19.97
_diffrn_reflns_theta_min         1.90
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.076
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.968
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             352
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .25
_exptl_crystal_size_min          .20
_refine_diff_density_max         1.271
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.125
_refine_ls_extinction_coef       0.022(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         1894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.493
_refine_ls_shift/su_mean         0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0594P)²+0.5908P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                1894
_reflns_number_total             1894
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b001384f.txt
_cod_data_source_block           vk02
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.5908P] 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^)+(0.0594P)^2^+0.5908P] 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        603.1(2)
_cod_database_code               7009482
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.0000 0.5000 0.5000 0.01966(16) Uani 1 d S . .
Rh2 Rh 0.0000 0.0000 0.0000 0.02050(16) Uani 1 d S . .
Cl1 Cl -0.18951(11) -0.03630(10) 0.22459(10) 0.0319(2) Uani 1 d . . .
Cl2 Cl -0.09105(11) 0.26247(10) 0.46566(10) 0.0323(2) Uani 1 d . . .
Cl3 Cl 0.23140(14) 0.47661(12) -0.02524(11) 0.0417(3) Uani 1 d . . .
O1 O 0.3186(3) 0.3440(3) 0.5573(3) 0.0361(6) Uani 1 d . . .
O2 O 0.2439(3) 0.0649(3) 0.1767(3) 0.0401(6) Uani 1 d . . .
N1 N 0.2047(4) 0.4330(4) 0.3452(4) 0.0264(6) Uani 1 d . . .
N2 N 0.1503(4) 0.3878(4) 0.6424(3) 0.0266(6) Uani 1 d . . .
N3 N 0.1754(4) -0.1525(4) 0.0794(4) 0.0287(6) Uani 1 d . . .
N4 N 0.0980(4) 0.1478(4) 0.1201(4) 0.0278(6) Uani 1 d . . .
C1 C 0.3295(4) 0.3676(4) 0.3999(4) 0.0310(8) Uani 1 d . . .
C2 C 0.4945(6) 0.3104(8) 0.3129(7) 0.0511(12) Uani 1 d . . .
C3 C 0.2692(4) -0.0936(5) 0.1509(5) 0.0347(8) Uani 1 d . . .
C4 C 0.4123(6) -0.1790(8) 0.2143(8) 0.0559(13) Uani 1 d . . .
H1N1 H 0.224(6) 0.454(6) 0.268(6) 0.045(15) Uiso 1 d . . .
H1N2 H 0.162(5) 0.445(5) 0.721(5) 0.033(11) Uiso 1 d . . .
H2N2 H 0.127(5) 0.292(5) 0.675(5) 0.030(10) Uiso 1 d . . .
H1N3 H 0.195(6) -0.249(6) 0.062(5) 0.042(12) Uiso 1 d . . .
H1N4 H 0.048(4) 0.173(4) 0.196(5) 0.012(9) Uiso 1 d . . .
H2N4 H 0.137(6) 0.223(6) 0.070(6) 0.036(12) Uiso 1 d . . .
H21 H 0.498(10) 0.213(11) 0.311(11) 0.11(3) Uiso 1 d . . .
H22 H 0.559(7) 0.357(7) 0.344(7) 0.070(19) Uiso 1 d . . .
H23 H 0.507(10) 0.351(9) 0.215(10) 0.10(3) Uiso 1 d . . .
H31 H 0.498(7) -0.140(7) 0.180(7) 0.060(16) Uiso 1 d . . .
H32 H 0.450(9) -0.278(10) 0.177(9) 0.11(3) Uiso 1 d . . .
H33 H 0.417(10) -0.155(10) 0.309(11) 0.12(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 0.0015 0.0009 '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 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -2.5280 0.5964 '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
N1 Rh1 N1 180.0 . 2_566 ?
N1 Rh1 N2 101.70(12) . 2_566 ?
N1 Rh1 N2 78.30(12) 2_566 2_566 ?
N1 Rh1 N2 78.30(12) . . ?
N1 Rh1 N2 101.70(12) 2_566 . ?
N2 Rh1 N2 180.0 2_566 . ?
N1 Rh1 Cl2 88.70(9) . 2_566 ?
N1 Rh1 Cl2 91.30(9) 2_566 2_566 ?
N2 Rh1 Cl2 90.56(10) 2_566 2_566 ?
N2 Rh1 Cl2 89.44(10) . 2_566 ?
N1 Rh1 Cl2 91.30(9) . . ?
N1 Rh1 Cl2 88.70(9) 2_566 . ?
N2 Rh1 Cl2 89.44(10) 2_566 . ?
N2 Rh1 Cl2 90.56(10) . . ?
Cl2 Rh1 Cl2 180.0 2_566 . ?
N3 Rh2 N3 180.0 2 . ?
N3 Rh2 N4 78.51(13) 2 2 ?
N3 Rh2 N4 101.49(13) . 2 ?
N3 Rh2 N4 101.49(13) 2 . ?
N3 Rh2 N4 78.51(13) . . ?
N4 Rh2 N4 180.0 2 . ?
N3 Rh2 Cl1 92.15(9) 2 2 ?
N3 Rh2 Cl1 87.85(9) . 2 ?
N4 Rh2 Cl1 90.40(10) 2 2 ?
N4 Rh2 Cl1 89.60(10) . 2 ?
N3 Rh2 Cl1 87.85(9) 2 . ?
N3 Rh2 Cl1 92.15(9) . . ?
N4 Rh2 Cl1 89.60(10) 2 . ?
N4 Rh2 Cl1 90.40(10) . . ?
Cl1 Rh2 Cl1 180.0 2 . ?
C1 O1 N2 111.9(3) . . ?
C3 O2 N4 112.3(3) . . ?
C1 N1 Rh1 117.5(3) . . ?
O1 N2 Rh1 112.08(19) . . ?
C3 N3 Rh2 117.1(3) . . ?
O2 N4 Rh2 111.8(2) . . ?
N1 C1 O1 119.5(3) . . ?
N1 C1 C2 128.4(4) . . ?
O1 C1 C2 112.1(4) . . ?
N3 C3 O2 119.7(3) . . ?
N3 C3 C4 127.7(4) . . ?
O2 C3 C4 112.5(4) . . ?
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 N1 2.002(3) . ?
Rh1 N1 2.002(3) 2_566 ?
Rh1 N2 2.029(3) 2_566 ?
Rh1 N2 2.029(3) . ?
Rh1 Cl2 2.3270(10) 2_566 ?
Rh1 Cl2 2.3270(10) . ?
Rh2 N3 2.006(3) 2 ?
Rh2 N3 2.006(3) . ?
Rh2 N4 2.025(3) 2 ?
Rh2 N4 2.025(3) . ?
Rh2 Cl1 2.3284(11) 2 ?
Rh2 Cl1 2.3284(11) . ?
O1 C1 1.353(5) . ?
O1 N2 1.476(4) . ?
O2 C3 1.350(5) . ?
O2 N4 1.472(4) . ?
N1 C1 1.271(5) . ?
N3 C3 1.264(5) . ?
C1 C2 1.476(6) . ?
C3 C4 1.489(6) . ?
