#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:43:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179986 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/80/7028063.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_7028063
loop_
_publ_author_name
'Steinborn, Dirk'
'Rausch, Mario'
'Bruhn, Clemens'
'Schmidt, Harry'
'Ströhl, Dieter'
_publ_section_title
;
 Syntheses and structures of novel cyclic and dinuclear organorhodoximes:
 a homologous series of di- to penta-methylene-bridged
 complexes ‡
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              221
_journal_paper_doi               10.1039/a706184f
_journal_year                    1998
_chemical_compound_source        'see text'
_chemical_formula_sum            'C62 H72 Cl18 N8 O8 P2 Rh2'
_chemical_formula_weight         1963.14
_chemical_melting_point          '240-245 \%C decomp.'
_chemical_name_systematic
; 

μ-butane-1,4-diyl-bis[bis(dimethylglyoximato-N,N')(triphenylphos
phine)
 rhodium(III)]
;
_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
_cell_angle_alpha                111.90(4)
_cell_angle_beta                 93.02(4)
_cell_angle_gamma                99.67(3)
_cell_formula_units_Z            1
_cell_length_a                   9.127(3)
_cell_length_b                   14.238(3)
_cell_length_c                   18.729(8)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    220(1)
_cell_volume                     2208.3(15)
_computing_cell_refinement
;
 Stoe IPDS-software (STOE publication 4805-010, 1996)
;
_computing_data_collection
;
 Stoe IPDS-software (STOE publication 4805-010, 1996)
;
_computing_data_reduction
;
 Stoe IPDS-software (STOE publication 4805-010, 1996)
;
_computing_molecular_graphics    'ORTEPIII (Johnson, C. K., 1997)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      220(1)
_diffrn_measurement_device       'STOE Image Plate Detection System'
_diffrn_measurement_method
;
The reciprocical space was scanned with 133 images each of which
with an exposure time of 5 min and a rotation angle of 1.5
degrees.
;
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_sigmaI/netI    0.0916
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15629
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         'max. 50 per image'
_exptl_absorpt_coefficient_mu    1.004
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate
_exptl_crystal_F_000             990
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.440
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.198
_refine_ls_extinction_coef       0.0118(23)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.128
_refine_ls_goodness_of_fit_obs   1.171
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.171
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_obs          0.0857
_refine_ls_shift/esd_max         0.009
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1467P)²+11.3960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2708
_refine_ls_wR_factor_obs         0.2617
_reflns_number_observed          6395
_reflns_number_total             7335
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            f706184csup1.cif
_cod_data_source_block           ipds220
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1467P)^2^+11.3960P] 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^)+(0.1467P)^2^+11.3960P] 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        2208.4(12)
_cod_database_code               7028063
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.0477(12) 0.4287(7) 0.2046(6) 0.049(2) Uani 1 d .
H1A H 0.1239(12) 0.4190(7) 0.1706(6) 0.058 Uiso 1 calc R
H1B H 0.0473(12) 0.5010(7) 0.2293(6) 0.058 Uiso 1 calc R
H1C H -0.0483(12) 0.3927(7) 0.1751(6) 0.058 Uiso 1 calc R
C2 C 0.0789(9) 0.3869(6) 0.2649(5) 0.037(2) Uani 1 d .
C3 C -0.0166(10) 0.3893(6) 0.3265(5) 0.038(2) Uani 1 d .
C4 C -0.1483(12) 0.4416(8) 0.3382(7) 0.056(2) Uani 1 d .
H4A H -0.1949(12) 0.4342(8) 0.3810(7) 0.067 Uiso 1 calc R
H4B H -0.2193(12) 0.4104(8) 0.2920(7) 0.067 Uiso 1 calc R
H4C H -0.1149(12) 0.5137(8) 0.3488(7) 0.067 Uiso 1 calc R
C5 C 0.5911(11) 0.1604(8) 0.3742(6) 0.052(2) Uani 1 d .
H5A H 0.6373(11) 0.1694(8) 0.3316(6) 0.062 Uiso 1 calc R
H5B H 0.5724(11) 0.0886(8) 0.3661(6) 0.062 Uiso 1 calc R
H5C H 0.6566(11) 0.1998(8) 0.4216(6) 0.062 Uiso 1 calc R
C6 C 0.4478(9) 0.1965(6) 0.3789(4) 0.034(2) Uani 1 d .
C7 C 0.3466(9) 0.1938(6) 0.4383(4) 0.033(2) Uani 1 d .
C8 C 0.3823(11) 0.1543(8) 0.4990(6) 0.051(2) Uani 1 d .
H8A H 0.3035(11) 0.1591(8) 0.5314(6) 0.061 Uiso 1 calc R
H8B H 0.4751(11) 0.1949(8) 0.5301(6) 0.061 Uiso 1 calc R
H8C H 0.3914(11) 0.0834(8) 0.4747(6) 0.061 Uiso 1 calc R
C9 C -0.0813(9) 0.0351(5) 0.2860(4) 0.031(2) Uani 1 d .
C10 C -0.1899(11) -0.0414(7) 0.2309(5) 0.049(2) Uani 1 d .
H10 H -0.1985(11) -0.0465(7) 0.1798(5) 0.058 Uiso 1 calc R
C11 C -0.2857(12) -0.1104(8) 0.2522(6) 0.066(3) Uani 1 d .
H11 H -0.3576(12) -0.1622(8) 0.2151(6) 0.079 Uiso 1 calc R
C12 C -0.2749(12) -0.1024(7) 0.3284(6) 0.056(3) Uani 1 d .
H12 H -0.3420(12) -0.1467(7) 0.3430(6) 0.067 Uiso 1 calc R
C13 C -0.1649(13) -0.0289(8) 0.3819(5) 0.055(3) Uani 1 d .
H13 H -0.1540(13) -0.0258(8) 0.4324(5) 0.066 Uiso 1 calc R
C14 C -0.0695(11) 0.0413(6) 0.3618(5) 0.043(2) Uani 1 d .
H14 H 0.0026(11) 0.0925(6) 0.3992(5) 0.052 Uiso 1 calc R
C15 C -0.0526(8) 0.1320(5) 0.1780(4) 0.0282(15) Uani 1 d .
C16 C -0.0149(11) 0.1093(7) 0.1027(4) 0.041(2) Uani 1 d .
H16 H 0.0684(11) 0.0803(7) 0.0882(4) 0.049 Uiso 1 calc R
C17 C -0.1030(13) 0.1302(8) 0.0494(5) 0.053(2) Uani 1 d .
H17 H -0.0760(13) 0.1171(8) 0.0000(5) 0.064 Uiso 1 calc R
C18 C -0.2298(12) 0.1701(7) 0.0694(5) 0.051(2) Uani 1 d .
H18 H -0.2888(12) 0.1827(7) 0.0332(5) 0.061 Uiso 1 calc R
C19 C -0.2683(10) 0.1911(7) 0.1429(5) 0.042(2) Uani 1 d .
H19 H -0.3537(10) 0.2177(7) 0.1566(5) 0.051 Uiso 1 calc R
C20 C -0.1776(9) 0.1721(6) 0.1978(4) 0.037(2) Uani 1 d .
H20 H -0.2032(9) 0.1870(6) 0.2477(4) 0.044 Uiso 1 calc R
C21 C 0.1780(9) 0.0246(6) 0.2075(4) 0.034(2) Uani 1 d .
C22 C 0.1663(13) -0.0718(8) 0.2137(6) 0.055(3) Uani 1 d .
H22 H 0.0929(13) -0.0930(8) 0.2403(6) 0.066 Uiso 1 calc R
C23 C 0.2640(17) -0.1346(9) 0.1804(8) 0.077(4) Uani 1 d .
H23 H 0.2559(17) -0.1980(9) 0.1851(8) 0.093 Uiso 1 calc R
C24 C 0.3737(14) -0.1062(9) 0.1400(6) 0.062(3) Uani 1 d .
H24 H 0.4372(14) -0.1506(9) 0.1172(6) 0.074 Uiso 1 calc R
C25 C 0.3889(11) -0.0112(7) 0.1338(5) 0.047(2) Uani 1 d .
H25 H 0.4638(11) 0.0092(7) 0.1077(5) 0.057 Uiso 1 calc R
C26 C 0.2913(10) 0.0528(6) 0.1667(4) 0.038(2) Uani 1 d .
H26 H 0.3008(10) 0.1161(6) 0.1618(4) 0.046 Uiso 1 calc R
C27 C 0.3193(10) 0.4322(6) 0.4280(5) 0.043(2) Uani 1 d .
H27A H 0.3318(10) 0.4773(6) 0.3997(5) 0.051 Uiso 1 calc R
H27B H 0.2530(10) 0.4581(6) 0.4663(5) 0.051 Uiso 1 calc R
C28 C 0.4693(9) 0.4447(5) 0.4712(4) 0.035(2) Uani 1 d .
H28A H 0.5400(9) 0.4242(5) 0.4342(4) 0.042 Uiso 1 calc R
H28B H 0.4605(9) 0.3989(5) 0.4989(4) 0.042 Uiso 1 calc R
C29 C -0.0853(14) 0.2380(8) 0.6072(6) 0.062(3) Uani 1 d .
H31 H -0.0125(14) 0.2183(8) 0.5705(6) 0.075 Uiso 1 calc R
C30 C 0.3096(16) 0.2518(10) 0.0324(7) 0.076(3) Uani 1 d .
H30 H 0.2736(16) 0.2688(10) 0.0832(7) 0.091 Uiso 1 calc R
C31 C 0.5067(15) 0.5573(10) 0.2358(10) 0.088(4) Uani 1 d .
H29 H 0.4447(15) 0.4878(10) 0.2194(10) 0.105 Uiso 1 calc R
N1 N 0.1923(7) 0.3432(4) 0.2674(4) 0.0320(14) Uani 1 d .
N2 N 0.0233(7) 0.3430(5) 0.3691(4) 0.0334(14) Uani 1 d .
N3 N 0.4000(7) 0.2397(4) 0.3339(3) 0.0285(13) Uani 1 d .
N4 N 0.2318(7) 0.2357(5) 0.4358(3) 0.0304(13) Uani 1 d .
O1 O 0.2948(6) 0.3354(4) 0.2173(3) 0.0372(13) Uani 1 d .
O2 O -0.0551(7) 0.3410(5) 0.4296(3) 0.0465(15) Uani 1 d .
H2 H -0.0176(7) 0.3091(5) 0.4517(3) 0.056 Uiso 1 calc R
O3 O 0.4894(6) 0.2567(4) 0.2811(3) 0.0373(12) Uani 1 d .
H3 H 0.4471(6) 0.2839(4) 0.2567(3) 0.045 Uiso 1 calc R
O4 O 0.1355(7) 0.2491(4) 0.4879(3) 0.0389(13) Uani 1 d .
P P 0.0607(2) 0.11496(13) 0.25515(10) 0.0257(4) Uani 1 d .
Cl1 Cl -0.1744(4) 0.3288(3) 0.5895(2) 0.0753(8) Uani 1 d .
Cl2 Cl -0.2251(5) 0.1261(3) 0.5946(2) 0.0993(13) Uani 1 d .
Cl3 Cl 0.0041(5) 0.2854(3) 0.7015(2) 0.0989(13) Uani 1 d .
Cl4 Cl 0.3258(4) 0.1246(3) -0.0020(2) 0.0779(9) Uani 1 d .
Cl5 Cl 0.4826(8) 0.3281(4) 0.0449(5) 0.183(3) Uani 1 d .
Cl6 Cl 0.1767(8) 0.2693(5) -0.0301(3) 0.140(2) Uani 1 d .
Cl7 Cl 0.6586(7) 0.5527(6) 0.1860(3) 0.157(3) Uani 1 d .
Cl8 Cl 0.3980(6) 0.6421(5) 0.2282(5) 0.165(3) Uani 1 d .
Cl9 Cl 0.5811(6) 0.6034(4) 0.3369(3) 0.1160(15) Uani 1 d .
Rh Rh 0.20663(6) 0.28420(4) 0.34859(3) 0.0240(3) Uani 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'
P P 0.1023 0.0942 '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_3
N1 C2 C3 113.3(7) .
N1 C2 C1 123.0(8) .
C3 C2 C1 123.6(8) .
N2 C3 C2 114.0(7) .
N2 C3 C4 123.3(8) .
C2 C3 C4 122.8(8) .
N3 C6 C5 123.5(8) .
N3 C6 C7 112.5(7) .
C5 C6 C7 123.9(7) .
N4 C7 C8 123.4(8) .
N4 C7 C6 114.2(6) .
C8 C7 C6 122.3(8) .
C14 C9 C10 119.4(7) .
C14 C9 P 120.6(6) .
C10 C9 P 119.5(6) .
C9 C10 C11 119.8(8) .
C12 C11 C10 120.4(8) .
C13 C12 C11 119.4(8) .
C12 C13 C14 120.8(8) .
C9 C14 C13 120.1(8) .
C20 C15 C16 119.5(7) .
C20 C15 P 116.7(5) .
C16 C15 P 123.8(7) .
C17 C16 C15 119.7(9) .
C18 C17 C16 120.8(8) .
C19 C18 C17 119.6(8) .
C18 C19 C20 119.9(9) .
C15 C20 C19 120.5(7) .
C22 C21 C26 117.8(8) .
C22 C21 P 122.1(7) .
C26 C21 P 120.0(6) .
C23 C22 C21 119.7(10) .
C22 C23 C24 121.9(10) .
C23 C24 C25 119.7(9) .
C26 C25 C24 119.3(9) .
C25 C26 C21 121.7(8) .
C28 C27 Rh 119.9(5) .
C27 C28 C28 112.9(8) 2_666
Cl3 C29 Cl1 111.9(6) .
Cl3 C29 Cl2 107.4(6) .
Cl1 C29 Cl2 108.5(7) .
Cl5 C30 Cl4 109.2(8) .
Cl5 C30 Cl6 113.6(9) .
Cl4 C30 Cl6 109.7(7) .
Cl7 C31 Cl8 114.8(9) .
Cl7 C31 Cl9 105.9(8) .
Cl8 C31 Cl9 106.6(8) .
C2 N1 O1 122.6(6) .
C2 N1 Rh 116.7(6) .
O1 N1 Rh 120.7(5) .
C3 N2 O2 119.8(7) .
C3 N2 Rh 117.7(6) .
O2 N2 Rh 122.3(5) .
C6 N3 O3 119.0(7) .
C6 N3 Rh 118.2(5) .
O3 N3 Rh 122.7(5) .
C7 N4 O4 123.4(6) .
C7 N4 Rh 116.3(5) .
O4 N4 Rh 120.2(5) .
C21 P C9 102.3(4) .
C21 P C15 106.9(3) .
C9 P C15 101.0(3) .
C21 P Rh 113.2(3) .
C9 P Rh 121.3(2) .
C15 P Rh 110.7(2) .
N3 Rh N2 174.4(2) .
N3 Rh N1 100.8(3) .
N2 Rh N1 78.2(3) .
N3 Rh N4 78.5(3) .
N2 Rh N4 102.1(3) .
N1 Rh N4 175.4(2) .
N3 Rh C27 90.0(3) .
N2 Rh C27 84.5(3) .
N1 Rh C27 88.7(3) .
N4 Rh C27 86.8(3) .
N3 Rh P 93.4(2) .
N2 Rh P 92.2(2) .
N1 Rh P 89.9(2) .
N4 Rh P 94.7(2) .
C27 Rh P 176.6(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C2 1.495(11) .
C2 N1 1.301(11) .
C2 C3 1.477(12) .
C3 N2 1.282(11) .
C3 C4 1.501(12) .
C5 C6 1.479(12) .
C6 N3 1.310(10) .
C6 C7 1.490(11) .
C7 N4 1.296(11) .
C7 C8 1.489(11) .
C9 C14 1.385(11) .
C9 C10 1.388(11) .
C9 P 1.839(8) .
C10 C11 1.388(12) .
C11 C12 1.386(14) .
C12 C13 1.366(14) .
C13 C14 1.386(12) .
C15 C20 1.368(12) .
C15 C16 1.399(10) .
C15 P 1.846(7) .
C16 C17 1.396(13) .
C17 C18 1.382(15) .
C18 C19 1.374(13) .
C19 C20 1.418(11) .
C21 C22 1.408(12) .
C21 C26 1.410(12) .
C21 P 1.817(8) .
C22 C23 1.377(15) .
C23 C24 1.38(2) .
C24 C25 1.385(15) .
C25 C26 1.384(12) .
C27 C28 1.502(11) .
C27 Rh 2.117(7) .
C28 C28 1.527(13) 2_666
C29 Cl3 1.736(12) .
C29 Cl1 1.757(12) .
C29 Cl2 1.796(12) .
C30 Cl5 1.71(2) .
C30 Cl4 1.716(13) .
C30 Cl6 1.752(15) .
C31 Cl7 1.71(2) .
C31 Cl8 1.73(2) .
C31 Cl9 1.81(2) .
N1 O1 1.348(9) .
N1 Rh 2.002(6) .
N2 O2 1.379(8) .
N2 Rh 1.987(7) .
N3 O3 1.379(8) .
N3 Rh 1.972(7) .
N4 O4 1.330(8) .
N4 Rh 2.013(6) .
P Rh 2.484(2) .
