#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/44/2224478.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# 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_2224478
loop_
_publ_author_name
'Venter, Johan A.'
'Purcell, W.'
'Visser, H. G.'
_publ_section_title
Di-μ-iodido-bis[acetyl(4-methyl-2,6,7-trioxa-1-phosphabicyclo[2.2.2]octane)(N-nitroso-N-oxidoaniline-κ²O,O')rhodium(III)]
_journal_coeditor_code           WM2267
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1528
_journal_page_last               m1529
_journal_paper_doi               10.1107/S1600536809043050
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac
'[Rh2 (C6 H5 N2 O2)2 (C2 H3 O)2 I2 (C5 H9 O3 P)2]'
_chemical_formula_moiety         'C26 H34 I2 N4 O12 P2 Rh2'
_chemical_formula_sum            'C26 H34 I2 N4 O12 P2 Rh2'
_chemical_formula_weight         1116.14
_chemical_name_systematic
;
Di-μ-iodido-bis[acetyl(4-methyl-2,6,7-trioxa-1-
phosphabicyclo[2.2.2]octane)(N-nitroso-N-oxidoaniline-
κ²O,O')rhodium(III)]
;
_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'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.055(2)
_cell_length_b                   16.944(3)
_cell_length_c                   11.149(2)
_cell_measurement_reflns_used    859
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      2.3
_cell_volume                     1751.7(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT-Plus (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART CCD 1K'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0506
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            12035
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.86
_exptl_absorpt_correction_T_max  0.8471
_exptl_absorpt_correction_T_min  0.763
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2004)
;
_exptl_crystal_colour            brown-red
_exptl_crystal_density_diffrn    2.116
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.495
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4344
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.95
_refine_ls_R_factor_gt           0.0327
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0354P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                3129
_reflns_number_total             4344
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            wm2267.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2224478
_cod_database_fobs_code          2224478
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C C6 0.3530(9) 0.3279(4) 0.4556(7) 0.0389(18) Uani d . 1 . .
C C5 0.3479(11) 0.2939(5) 0.5784(8) 0.053(2) Uani d . 1 . .
H H1A 0.4329 0.3102 0.6522 0.064 Uiso calc R 1 . .
H H1B 0.2637 0.314 0.5908 0.064 Uiso calc R 1 . .
C C4 0.4801(10) 0.2932(5) 0.4347(9) 0.050(2) Uani d . 1 . .
H H2A 0.4849 0.3154 0.3563 0.06 Uiso calc R 1 . .
H H2B 0.568 0.3073 0.5072 0.06 Uiso calc R 1 . .
C C7 0.3688(11) 0.4178(5) 0.4674(9) 0.060(3) Uani d . 1 . .
H H5A 0.4549 0.431 0.5408 0.091 Uiso calc R 1 . .
H H5B 0.2867 0.4399 0.479 0.091 Uiso calc R 1 . .
H H5C 0.3747 0.4389 0.3897 0.091 Uiso calc R 1 . .
O O1 0.1009(7) 0.0872(4) 0.5202(7) 0.0698(19) Uani d . 1 . .
C C1 0.1039(9) 0.0605(5) 0.4219(9) 0.045(2) Uani d . 1 . .
C C2 -0.0248(11) 0.0383(7) 0.3093(10) 0.074(3) Uani d . 1 . .
H H9A -0.0107 -0.0129 0.279 0.111 Uiso calc R 1 . .
H H9B -0.0418 0.0763 0.2412 0.111 Uiso calc R 1 . .
H H9C -0.1064 0.0366 0.3338 0.111 Uiso calc R 1 . .
I I 0.43362(5) -0.00049(3) 0.64352(4) 0.03779(16) Uani d . 1 . .
Rh Rh 0.29476(7) 0.04485(4) 0.40073(6) 0.03779(16) Uani d U 1 . .
P P 0.3320(2) 0.17126(11) 0.43763(19) 0.0342(4) Uani d . 1 . .
O O2 0.2452(6) -0.0699(3) 0.3412(5) 0.0382(12) Uani d . 1 . .
N N1 0.1775(7) -0.0076(4) 0.1406(6) 0.0433(16) Uani d . 1 . .
O O3 0.2017(6) 0.0583(3) 0.2034(5) 0.0413(13) Uani d . 1 . .
N N2 0.1995(7) -0.0702(3) 0.2114(6) 0.0366(14) Uani d . 1 . .
C C11 0.1793(8) -0.1465(4) 0.1476(7) 0.0355(17) Uani d . 1 . .
O O6 0.4702(6) 0.2079(3) 0.4228(6) 0.0495(14) Uani d . 1 . .
O O4 0.2045(6) 0.2201(3) 0.3337(5) 0.0511(15) Uani d . 1 . .
O O5 0.3416(7) 0.2073(3) 0.5719(5) 0.0535(16) Uani d . 1 . .
C C15 0.2426(11) -0.2819(5) 0.1644(10) 0.061(3) Uani d . 1 . .
H H010 0.292 -0.3249 0.2131 0.073 Uiso calc R 1 . .
C C16 0.2521(10) -0.2091(5) 0.2224(8) 0.050(2) Uani d . 1 . .
H H011 0.3069 -0.2026 0.3107 0.061 Uiso calc R 1 . .
C C13 0.0867(11) -0.2264(6) -0.0368(10) 0.068(3) Uani d . 1 . .
H H012 0.0298 -0.2321 -0.1248 0.082 Uiso calc R 1 . .
C C12 0.0962(10) -0.1545(5) 0.0197(8) 0.058(2) Uani d . 1 . .
H H013 0.0463 -0.1114 -0.0288 0.07 Uiso calc R 1 . .
C C14 0.1587(11) -0.2907(6) 0.0322(10) 0.065(3) Uani d . 1 . .
H H014 0.1518 -0.3393 -0.0083 0.078 Uiso calc R 1 . .
C C3 0.2178(10) 0.3068(4) 0.3415(9) 0.051(2) Uani d . 1 . .
H H01A 0.1346 0.3297 0.3522 0.061 Uiso calc R 1 . .
H H01B 0.2222 0.3275 0.262 0.061 Uiso calc R 1 . .
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C5 C6 C4 . . 108.7(7) ?
C5 C6 C3 . . 110.0(7) ?
C4 C6 C3 . . 108.7(7) ?
C5 C6 C7 . . 110.0(6) ?
C4 C6 C7 . . 109.6(7) ?
C3 C6 C7 . . 109.8(6) ?
O5 C5 C6 . . 110.7(6) ?
O5 C5 H1A . . 109.5 ?
C6 C5 H1A . . 109.5 ?
O5 C5 H1B . . 109.5 ?
C6 C5 H1B . . 109.5 ?
H1A C5 H1B . . 108.1 ?
O6 C4 C6 . . 111.8(6) ?
O6 C4 H2A . . 109.3 ?
C6 C4 H2A . . 109.3 ?
O6 C4 H2B . . 109.3 ?
C6 C4 H2B . . 109.3 ?
H2A C4 H2B . . 107.9 ?
C6 C7 H5A . . 109.5 ?
C6 C7 H5B . . 109.5 ?
H5A C7 H5B . . 109.5 ?
C6 C7 H5C . . 109.5 ?
H5A C7 H5C . . 109.5 ?
H5B C7 H5C . . 109.5 ?
O1 C1 C2 . . 123.8(9) ?
O1 C1 Rh . . 120.9(7) ?
C2 C1 Rh . . 115.3(7) ?
C1 C2 H9A . . 109.5 ?
C1 C2 H9B . . 109.5 ?
H9A C2 H9B . . 109.5 ?
C1 C2 H9C . . 109.5 ?
H9A C2 H9C . . 109.5 ?
H9B C2 H9C . . 109.5 ?
Rh I Rh . 3_656 93.30(2) y
C1 Rh O3 . . 92.9(3) y
C1 Rh O2 . . 92.2(3) y
O3 Rh O2 . . 78.74(19) y
C1 Rh P . . 87.2(2) ?
O3 Rh P . . 93.85(14) ?
O2 Rh P . . 172.54(15) y
C1 Rh I . . 93.9(2) y
O3 Rh I . . 168.12(14) y
O2 Rh I . . 91.25(14) ?
P Rh I . . 96.21(6) ?
C1 Rh I . 3_656 172.7(2) y
O3 Rh I . 3_656 85.36(16) ?
O2 Rh I . 3_656 80.51(15) ?
P Rh I . 3_656 99.96(6) ?
I Rh I . 3_656 86.70(2) ?
O6 P O5 . . 102.2(3) ?
O6 P O4 . . 102.2(3) ?
O5 P O4 . . 103.0(3) ?
O6 P Rh . . 117.2(2) ?
O5 P Rh . . 120.0(2) ?
O4 P Rh . . 110.0(2) ?
N2 O2 Rh . . 107.0(4) ?
O3 N1 N2 . . 115.4(6) ?
N1 O3 Rh . . 113.5(4) ?
N1 N2 O2 . . 124.3(6) ?
N1 N2 C11 . . 118.3(6) ?
O2 N2 C11 . . 117.3(6) ?
C12 C11 C16 . . 122.0(7) ?
C12 C11 N2 . . 121.2(7) ?
C16 C11 N2 . . 116.7(7) ?
C4 O6 P . . 114.3(5) ?
C3 O4 P . . 116.6(5) ?
C5 O5 P . . 114.7(4) ?
C16 C15 C14 . . 119.7(9) ?
C16 C15 H010 . . 120.2 ?
C14 C15 H010 . . 120.2 ?
C11 C16 C15 . . 118.8(8) ?
C11 C16 H011 . . 120.6 ?
C15 C16 H011 . . 120.6 ?
C14 C13 C12 . . 121.8(9) ?
C14 C13 H012 . . 119.1 ?
C12 C13 H012 . . 119.1 ?
C11 C12 C13 . . 118.9(9) ?
C11 C12 H013 . . 120.6 ?
C13 C12 H013 . . 120.6 ?
C13 C14 C15 . . 118.8(8) ?
C13 C14 H014 . . 120.6 ?
C15 C14 H014 . . 120.6 ?
O4 C3 C6 . . 108.6(6) ?
O4 C3 H01A . . 110 ?
C6 C3 H01A . . 110 ?
O4 C3 H01B . . 110 ?
C6 C3 H01B . . 110 ?
H01A C3 H01B . . 108.4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C6 C5 . 1.504(10) ?
C6 C4 . 1.504(11) ?
C6 C3 . 1.502(12) ?
C6 C7 . 1.533(10) ?
C5 O5 . 1.468(9) ?
C5 H1A . 0.97 ?
C5 H1B . 0.97 ?
C4 O6 . 1.451(8) ?
C4 H2A . 0.97 ?
C4 H2B . 0.97 ?
C7 H5A . 0.96 ?
C7 H5B . 0.96 ?
C7 H5C . 0.96 ?
O1 C1 . 1.196(10) ?
C1 C2 . 1.461(13) ?
C1 Rh . 2.040(8) y
C2 H9A . 0.96 ?
C2 H9B . 0.96 ?
C2 H9C . 0.96 ?
I Rh . 2.6351(8) y
I Rh 3_656 3.0511(9) ?
Rh O3 . 2.044(5) y
Rh O2 . 2.052(5) y
Rh P . 2.186(2) y
Rh I 3_656 3.0511(9) y
P O6 . 1.588(6) y
P O5 . 1.585(5) y
P O4 . 1.589(5) ?
O2 N2 . 1.339(7) ?
N1 O3 . 1.290(8) ?
N1 N2 . 1.289(8) ?
N2 C11 . 1.451(9) ?
C11 C12 . 1.352(10) ?
C11 C16 . 1.374(11) ?
O4 C3 . 1.474(9) ?
C15 C16 . 1.379(11) ?
C15 C14 . 1.394(13) ?
C15 H010 . 0.93 ?
C16 H011 . 0.93 ?
C13 C14 . 1.368(14) ?
C13 C12 . 1.358(12) ?
C13 H012 . 0.93 ?
C12 H013 . 0.93 ?
C14 H014 . 0.93 ?
C3 H01A . 0.97 ?
C3 H01B . 0.97 ?
