# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2005


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Marina Petrukhina'
'Vladimir V. Chernyshev'
'Evgeny V. Dikarev'
'Bo Li.'
'Roman V. Shpanchenko'

_publ_contact_author_name        'Dr Marina Petrukhina'
_publ_contact_author_address     
;
Department of Chemistry
University at Albany
1400 Washington Avenue
Albany
NY
12222
UNITED STATES OF AMERICA
;

_publ_contact_author_email       MARINA@ALBANY.EDU

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Coordination Polymers Formed in Solution and in
Solvent-Free Environment. Structural Transformation due to Interstitial
Solvent Removal Revealed by X-ray Powder Diffraction
;

data_Rh2(O2CCF3)4(C6H4(CN)2)
_database_code_depnum_ccdc_archive 'CCDC 266399'

#-------------------------------------------------------------------------
# 1. References

_publ_section_references         
;
Ahtee, M., Nurmela, M., Suortti, P. & Jarvinen, M. (1989).
J. Appl. Cryst. 22, 261-268.

Chernyshev, V. V. & Schenk, H. (1998). Z. Kristallogr. 213, 1--3.

Jarvinen, M. (1993). J. Appl. Cryst. 26, 525-531.

Nardelli, M. (1983). Comput. Chem. 7, 95--98.

Sheldrick, G. M. (1997). SHELXL97. Program for the refinement of crystal
structures. University of G\"ottingen, Germany.

Spek, A. L. (1992). PLUTON-92. Program for the viewing, analysis and
presentation of molecular structures. University of Utrecht, The Netherlands.

Toraya, H. (1986). J. Appl. Cryst. 19, 440-447.

Zlokazov, V. B. & Chernyshev, V. V. (1992). J. Appl. Cryst. 25, 447--451.
;

#-------------------------------------------------------------------------
# 2. Other data relating to the structure determination and refinement

# Record the radiation type if not X-rays, eg. neutron
# Record the temperature of the data collection (Kelvin)
# if not room-temperature
# Record R_squared if this is the only reliability factor given by
# your refinement program
# Describe briefly any disorder, eg. t-Butyl C31-33 disordered over
# two sites with occupancies 0.6 and 0.4
# Under ccdc_comments record any other important information

_diffrn_radiation_type           Cu
_diffrn_measurement_device       'Stoe STADI-P'
_ccdc_temp_data_collection       293(2)
_ccdc_ls_R_squared               ?
_refine_ls_abs_structure_details ?
_ccdc_disorder                   ?
_ccdc_comments                   ?

#-------------------------------------------------------------------------
# 3. Include your "standard" CIF file here
# It should contain the following data items:
# unit cell parameters and volume, z value, space group symbol,
# R-factor(s), atomic coordinates with standard deviations,
# occupancy factors, bond lengths and bond angles
# Other data items may be present but will not necessarily be
# included in the Cambridge Structural Database
# Do not include structure factors

_audit_creation_method           ?
_chemical_name_systematic        
;
Catena-[tetrakis(mu-trifluoroacetato-O,O')dirhodium(II,II)-
(1,3-dicyanobenzene-N,N')]
;
_chemical_name_common            ?
_chemical_formula_moiety         
;
[Rh2 (O2 C C F3)4 (C6 H4 (CN)2)]
;
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_sum            'C16 H4 F12 N2 O8 Rh2'
_chemical_formula_weight         786.03
_chemical_melting_point          '603 (decomposition)'
_chemical_compound_source        synthesized

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 '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'

# 4. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y, -z-1/2'
'-x+1/2, -y+1/2, -z'
'-x+1/2, y+1/2, -z-1/2'

_cell_length_a                   19.411(20)
_cell_length_b                   16.879(19)
_cell_length_c                   8.348(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 114.91(2)
_cell_angle_gamma                90.00
_cell_volume                     2481(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    2.105
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1504

_pd_char_particle_morphology     ?
_pd_char_colour                  purple

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min. The pressure at which the sample was
# prepared is in kPa. The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             358

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    12.060
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#==============================================================================
# 5. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
;
?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
;
?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
;
STADI/P STOE Department of Chemistry, MSU, Moscow 119992, Russia
;
_pd_calibration_special_details  # description of the method used

; # to calibrate the instrument
Si external standard
;
_diffrn_ambient_temperature      293
_diffrn_source                   'sealed X-Ray tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Cu K\a~1~'
_diffrn_measurement_device_type  'STADI/P STOE'
_diffrn_detector                 PSD
_diffrn_detector_type            'linear PSD'
# make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;
?
;

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  'Ge primiry beam'

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          260
_pd_instr_dist_mono/spec         130
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         130

# 6. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              5 # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
;
mylar foil
;
_pd_spec_mount_mode              transmission # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   flat_sheet # options are 'cylinder'
# 'flat_sheet' or 'irregular'

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        5901
_pd_meas_2theta_range_min        6.00
_pd_meas_2theta_range_max        65.00
_pd_meas_2theta_range_inc        0.01

# The following fields are used to identify the programs used.

_computing_data_collection       'Stoe STADI-P program package'
_computing_cell_refinement       'local program'
_computing_data_reduction        'local program'
_computing_structure_solution    'MRIA (Chernyshev & Zlokazov, 1992)'
_computing_structure_refinement  MRIA
_computing_molecular_graphics    'PLUTON92 (Spek, 1992)'
_computing_publication_material  
;
MRIA, SHELXL97 (Sheldrick, 1997), PARST (Nardelli, 1983)
;

#==============================================================================

# 7. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
?
;

# The next three items are given as text
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_background_function  
;
Chebyshev polynomial up to the 5th order
;
_pd_proc_ls_pref_orient_corr     
;
Symmetrized harmonics expansion up to the 4th order (Ahtee et al., 1989,
Jarvinen, 1993)
;

_pd_proc_ls_prof_R_factor        0.0324
_pd_proc_ls_prof_wR_factor       0.0426
_pd_proc_ls_prof_wR_expected     0.0342

_refine_special_details          
;
?
;

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    calc
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     118
_refine_ls_number_restraints     73
_refine_ls_number_constraints    5

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.246

_refine_ls_restrained_S_all      1.246
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          .01
_refine_ls_shift/su_mean         .003
_refine_diff_density_max         0.78
_refine_diff_density_min         -0.83

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min        6
_pd_proc_2theta_range_max        65
_pd_proc_2theta_range_inc        0.01

_pd_proc_wavelength              1.5406

_pd_block_diffractogram_id       RSh_5_pattern # The id used for the block
# containing the powder
# pattern profile (section 11).

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
_atom_site_disorder_group
Rh Rh 0.2861(3) 0.2942(3) 0.4526(7) 0.025(4) Uiso 1 d . .
O1 O 0.1862(17) 0.3174(20) 0.242(4) 0.051 Uiso 1 d . .
O2 O 0.3805(16) 0.265(2) 0.672(5) 0.051 Uiso 1 d . .
O3 O 0.3032(17) 0.202(3) 0.317(3) 0.051 Uiso 1 d . .
O4 O 0.2637(19) 0.3816(17) 0.595(5) 0.051 Uiso 1 d . .
C1 C 0.127(2) 0.283(4) 0.225(6) 0.051 Uiso 1 d . .
C2 C 0.276(3) 0.133(3) 0.324(6) 0.051 Uiso 1 d . .
C3 C 0.056(3) 0.307(4) 0.059(6) 0.051 Uiso 1 d . .
C4 C 0.296(3) 0.069(3) 0.224(6) 0.051 Uiso 1 d . .
F1 F -0.0036(18) 0.271(2) 0.053(4) 0.193(18) Uiso 1 d . .
F2 F 0.0655(17) 0.289(2) -0.085(5) 0.193(18) Uiso 1 d . .
F3 F 0.0446(20) 0.3839(19) 0.056(5) 0.193(18) Uiso 1 d . .
F4 F 0.3346(19) 0.0991(20) 0.139(5) 0.193(18) Uiso 1 d . .
F5 F 0.235(2) 0.0352(20) 0.105(6) 0.193(18) Uiso 1 d . .
F6 F 0.3390(19) 0.014(3) 0.330(5) 0.193(18) Uiso 1 d . .
N1 N 0.346(2) 0.377(2) 0.351(5) 0.051 Uiso 1 d . .
C5 C 0.388(2) 0.411(3) 0.314(7) 0.051 Uiso 1 d . .
C6 C 0.5000 0.413(5) 0.2500 0.051 Uiso 1 d S .
C7 C 0.446(3) 0.454(3) 0.283(7) 0.051 Uiso 1 d . .
C8 C 0.446(3) 0.536(3) 0.284(8) 0.051 Uiso 1 d . .
C9 C 0.5000 0.577(5) 0.2500 0.051 Uiso 1 d S .
H6 H 0.5000 0.3580 0.2500 0.051 Uiso 1 d S .
H8 H 0.4100 0.5630 0.3070 0.051 Uiso 1 d . .
H9 H 0.5000 0.6320 0.2500 0.051 Uiso 1 d S .

_geom_special_details            
;
All esds
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry.
;

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
Rh O2 2.03(4) . y
Rh O3 2.03(4) . y
Rh O1 2.03(4) . y
Rh O4 2.05(4) . y
Rh N1 2.20(5) . y
Rh Rh 2.398(9) 7_556 y
O1 C1 1.24(6) . ?
O2 C1 1.23(6) 7_556 ?
O3 C2 1.29(7) . ?
O4 C2 1.25(6) 7_556 ?
C1 O2 1.23(6) 7_556 ?
C1 C3 1.54(6) . ?
C2 O4 1.25(6) 7_556 ?
C2 C4 1.51(8) . ?
C3 F1 1.29(7) . ?
C3 F3 1.32(7) . ?
C3 F2 1.33(7) . ?
C4 F6 1.31(6) . ?
C4 F5 1.31(6) . ?
C4 F4 1.33(8) . ?
N1 C5 1.14(7) . y
C5 C7 1.45(8) . ?
C6 C7 1.38(8) . ?
C6 C7 1.38(8) 6_656 ?
C6 H6 0.93 . ?
C7 C8 1.38(8) . ?
C8 C9 1.38(8) . ?
C8 H8 0.92 . ?
C9 C8 1.38(8) 6_656 ?
C9 H9 0.93 . ?

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
O2 Rh O3 91(2) . . y
O2 Rh O1 175(2) . . y
O3 Rh O1 89(2) . . y
O2 Rh O4 89(2) . . y
O3 Rh O4 176(2) . . y
O1 Rh O4 90(2) . . y
O2 Rh N1 95(2) . . y
O3 Rh N1 92(2) . . y
O1 Rh N1 91(2) . . y
O4 Rh N1 92(2) . . y
O2 Rh Rh 89(1) . 7_556 y
O3 Rh Rh 88(1) . 7_556 y
O1 Rh Rh 86(1) . 7_556 y
O4 Rh Rh 88(1) . 7_556 y
N1 Rh Rh 177(1) . 7_556 y
C1 O1 Rh 121(3) . . ?
C1 O2 Rh 118(3) 7_556 . ?
C2 O3 Rh 120(3) . . ?
C2 O4 Rh 120(3) 7_556 . ?
O2 C1 O1 127(4) 7_556 . ?
O2 C1 C3 118(4) 7_556 . ?
O1 C1 C3 115(4) . . ?
O4 C2 O3 124(4) 7_556 . ?
O4 C2 C4 121(4) 7_556 . ?
O3 C2 C4 115(4) . . ?
F1 C3 F3 109(5) . . ?
F1 C3 F2 109(5) . . ?
F3 C3 F2 107(5) . . ?
F1 C3 C1 111(4) . . ?
F3 C3 C1 111(4) . . ?
F2 C3 C1 110(4) . . ?
F6 C4 F5 109(4) . . ?
F6 C4 F4 107(4) . . ?
F5 C4 F4 107(4) . . ?
F6 C4 C2 112(4) . . ?
F5 C4 C2 112(4) . . ?
F4 C4 C2 111(4) . . ?
C5 N1 Rh 168(3) . . y
N1 C5 C7 175(5) . . y
C7 C6 C7 120(5) . 6_656 ?
C7 C6 H6 120 . . ?
C7 C6 H6 120 6_656 . ?
C6 C7 C8 120(5) . . ?
C6 C7 C5 120(5) . . ?
C8 C7 C5 120(5) . . ?
C9 C8 C7 120(5) . . ?
C9 C8 H8 120 . . ?
C7 C8 H8 120 . . ?
C8 C9 C8 120(5) . 6_656 ?
C8 C9 H9 120 . . ?
C8 C9 H9 120 6_656 . ?

data_Rh2(O2CCF3)4(C6H4(CN)2)_7/4(C6H6)_1/2(CH2Cl2)
_database_code_depnum_ccdc_archive 'CCDC 266400'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
Catena-[tetrakis(mu-trifluoroacetato-O,O')dirhodium(II,II)-
(1,3-dicyanobenzene-N,N')], benzene solvate, dichloromethane
solvate
;
_chemical_melting_point          'not measured'
_chemical_formula_moiety         
;
'[Rh2 (O2 C C F3)4 (C6 H4 (CN)2)] (C6 H6)7/4 (C H2 Cl2)1/2'
;
_chemical_formula_sum            'C27 H15.50 Cl F12 N2 O8 Rh2'
_chemical_formula_weight         965.18

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'
F F 0.0171 0.0103 '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'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n m a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   16.3302(10)
_cell_length_b                   24.7253(15)
_cell_length_c                   8.7079(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3516.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6738
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      28.29

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    none
_exptl_crystal_F_000             1882
_exptl_absorpt_coefficient_mu    1.126
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_absorpt_correction_T_min  0.8062
_exptl_absorpt_correction_T_max  0.9355

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         'none (area detector data)'
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_decay_%        0
_diffrn_reflns_number            28857
_diffrn_reflns_av_R_equivalents  0.0172
_diffrn_reflns_av_sigmaI/netI    0.0121
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.48
_diffrn_reflns_theta_max         28.32
_reflns_number_total             4260
_reflns_number_gt                3849
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       SMART
_computing_cell_refinement       'SMART, SAINT'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+15.5520P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       na
_refine_ls_number_reflns         4260
_refine_ls_number_parameters     266
_refine_ls_number_restraints     50
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1437
_refine_ls_wR_factor_gt          0.1405
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.02729(2) 0.960184(13) 0.93829(4) 0.02916(13) Uani 1 1 d . . .
O1 O -0.0884(2) 0.94291(14) 0.8680(4) 0.0386(7) Uani 1 1 d . A .
O2 O 0.0075(2) 0.91909(13) 1.1383(4) 0.0387(7) Uani 1 1 d . B .
O3 O 0.1395(2) 0.98211(14) 1.0198(4) 0.0407(8) Uani 1 1 d . . .
O4 O 0.0436(2) 1.00636(13) 0.7466(4) 0.0374(7) Uani 1 1 d . . .
N1 N 0.0759(3) 0.88749(15) 0.8253(5) 0.0395(9) Uani 1 1 d . . .
C1 C -0.1432(3) 0.9757(2) 0.9029(6) 0.0415(11) Uani 1 1 d . . .
C2 C -0.2291(4) 0.9605(3) 0.8426(9) 0.0676(19) Uani 1 1 d D A 1
F1 F -0.2850(8) 0.9591(7) 0.9530(14) 0.089(4) Uiso 0.40 1 d PD A 1
F2 F -0.2572(9) 1.0047(5) 0.7574(18) 0.079(3) Uiso 0.40 1 d PD A 1
F3 F -0.2317(6) 0.9158(4) 0.7613(14) 0.056(2) Uiso 0.40 1 d PD A 1
F1X F -0.2640(7) 0.9297(5) 0.9568(11) 0.071(3) Uiso 0.40 1 d PD A 2
F2X F -0.2783(8) 1.0028(4) 0.8265(19) 0.078(3) Uiso 0.40 1 d PD A 2
F3X F -0.2279(6) 0.9347(5) 0.7107(12) 0.067(3) Uiso 0.40 1 d PD A 2
F1Y F -0.2883(10) 0.9866(9) 0.914(2) 0.056(4) Uiso 0.20 1 d PD A 3
F2Y F -0.2289(16) 0.9811(11) 0.696(2) 0.088(7) Uiso 0.20 1 d PD A 3
F3Y F -0.2443(14) 0.9091(6) 0.836(3) 0.073(6) Uiso 0.20 1 d PD A 3
C3 C -0.0214(3) 0.9455(2) 1.2476(6) 0.0380(10) Uani 1 1 d . . .
C4 C -0.0287(5) 0.9146(3) 1.4004(8) 0.068(2) Uani 1 1 d D B 1
F4 F 0.0480(6) 0.9061(7) 1.4561(15) 0.074(4) Uiso 0.40 1 d PD B 1
F5 F -0.0582(8) 0.8638(4) 1.3762(12) 0.062(2) Uiso 0.40 1 d PD B 1
F6 F -0.0723(9) 0.9398(5) 1.5038(12) 0.045(3) Uiso 0.40 1 d PD B 1
F4X F 0.0479(7) 0.9247(7) 1.4758(17) 0.060(4) Uiso 0.30 1 d PD B 2
F5X F -0.0197(8) 0.8603(4) 1.3879(12) 0.039(2) Uiso 0.30 1 d PD B 2
F6X F -0.0891(8) 0.9267(6) 1.4866(17) 0.060(5) Uiso 0.30 1 d PD B 2
F4Y F 0.0207(12) 0.8749(8) 1.422(2) 0.091(5) Uiso 0.30 1 d PD B 3
F5Y F -0.1033(9) 0.8839(7) 1.3708(19) 0.082(4) Uiso 0.30 1 d PD B 3
F6Y F -0.0461(11) 0.9414(7) 1.5180(17) 0.067(5) Uiso 0.30 1 d PD B 3
C5 C 0.0964(3) 0.84843(17) 0.7692(5) 0.0347(9) Uani 1 1 d . . .
C6 C 0.1219(3) 0.79816(17) 0.6998(5) 0.0332(9) Uani 1 1 d . . .
C7 C 0.1702(3) 0.79825(19) 0.5684(6) 0.0410(11) Uani 1 1 d . . .
H7 H 0.1866 0.8315 0.5233 0.049 Uiso 1 1 calc R . .
C8 C 0.1943(6) 0.7500 0.5035(9) 0.0487(19) Uani 1 2 d S . .
H8 H 0.2276 0.7500 0.4141 0.058 Uiso 1 2 calc SR . .
C9 C 0.0974(4) 0.7500 0.7666(8) 0.0339(13) Uani 1 2 d S . .
H9 H 0.0645 0.7500 0.8565 0.041 Uiso 1 2 calc SR . .
C10 C 0.256(4) 0.3741(16) 0.622(5) 0.056(16) Uiso 0.13 1 d PD . 1
H10A H 0.2202 0.3832 0.5334 0.067 Uiso 0.13 1 calc PR . 1
H10B H 0.3016 0.4002 0.6250 0.067 Uiso 0.13 1 calc PR . 1
Cl1 Cl 0.2925(10) 0.3091(5) 0.6039(15) 0.050(3) Uiso 0.13 1 d PD . 1
Cl2 Cl 0.1997(8) 0.3768(5) 0.7930(13) 0.046(3) Uiso 0.13 1 d PD . 1
C10X C 0.279(3) 0.3797(11) 0.638(4) 0.030(9) Uiso 0.13 1 d PD C 2
H10C H 0.2656 0.4069 0.5580 0.036 Uiso 0.13 1 calc PR C 2
H10D H 0.3374 0.3830 0.6635 0.036 Uiso 0.13 1 calc PR C 2
Cl1X Cl 0.2593(11) 0.3160(7) 0.5679(18) 0.069(4) Uiso 0.13 1 d PD C 2
Cl2X Cl 0.2198(8) 0.3920(5) 0.8010(13) 0.047(3) Uiso 0.13 1 d PD C 2
C11 C 0.0994(16) 0.2500 0.003(3) 0.081(6) Uiso 0.50 2 d SPD . 1
H11 H 0.0981 0.2500 -0.1064 0.097 Uiso 0.50 2 calc SPR . 1
C12 C 0.1003(8) 0.2996(5) 0.077(2) 0.053(3) Uiso 0.50 1 d PD . 1
H12 H 0.0943 0.3329 0.0242 0.064 Uiso 0.50 1 calc PR . 1
C13 C 0.1103(11) 0.2967(6) 0.232(2) 0.078(5) Uiso 0.50 1 d PD . 1
H13 H 0.1152 0.3297 0.2877 0.094 Uiso 0.50 1 calc PR . 1
C14 C 0.114(2) 0.2500 0.313(4) 0.104(9) Uiso 0.50 2 d SPD . 1
H14 H 0.1185 0.2500 0.4216 0.125 Uiso 0.50 2 calc SPR . 1
C11X C 0.070(2) 0.2500 -0.074(3) 0.103(9) Uiso 0.50 2 d SPD . 2
H11X H 0.0535 0.2500 -0.1781 0.123 Uiso 0.50 2 calc SPR . 2
C12X C 0.0828(11) 0.2960(7) 0.004(2) 0.083(5) Uiso 0.50 1 d PD . 2
H12X H 0.0752 0.3292 -0.0489 0.100 Uiso 0.50 1 calc PR . 2
C13X C 0.1057(9) 0.2978(6) 0.154(2) 0.061(3) Uiso 0.50 1 d PD . 2
H13X H 0.1137 0.3315 0.2041 0.073 Uiso 0.50 1 calc PR . 2
C14X C 0.117(2) 0.2500 0.233(4) 0.104(10) Uiso 0.50 2 d SPD . 2
H14X H 0.1324 0.2500 0.3386 0.125 Uiso 0.50 2 calc SPR . 2
C15 C 0.3956(10) 0.2787(3) 0.6596(18) 0.124(5) Uiso 0.75 1 d PD . .
H15 H 0.4465 0.2954 0.6829 0.148 Uiso 0.75 1 calc PR . .
C16 C 0.3322(7) 0.3130(4) 0.6305(12) 0.071(3) Uiso 0.75 1 d PD . .
H16 H 0.3340 0.3514 0.6345 0.085 Uiso 0.75 1 calc PR . .
C17 C 0.2598(11) 0.2796(3) 0.592(2) 0.138(6) Uiso 0.75 1 d PD . .
H17 H 0.2105 0.2976 0.5650 0.165 Uiso 0.75 1 calc PR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Rh1 0.0330(2) 0.02296(19) 0.0315(2) -0.00303(12) 0.00057(13) 0.00010(12)
O1 0.0388(17) 0.0344(16) 0.0426(18) -0.0067(14) -0.0040(15) -0.0080(14)
O2 0.0513(19) 0.0292(16) 0.0358(17) 0.0026(13) 0.0038(15) 0.0027(14)
O3 0.0320(16) 0.0418(19) 0.0484(19) -0.0030(16) -0.0045(15) 0.0034(14)
O4 0.0458(18) 0.0337(16) 0.0326(16) -0.0008(14) 0.0060(14) -0.0017(14)
N1 0.052(2) 0.0227(18) 0.044(2) -0.0012(16) 0.0058(19) -0.0032(16)
C1 0.041(3) 0.044(3) 0.040(2) 0.000(2) -0.005(2) -0.007(2)
C2 0.050(3) 0.080(5) 0.073(5) -0.013(4) -0.005(3) -0.008(3)
C3 0.043(3) 0.035(2) 0.036(2) 0.001(2) -0.004(2) -0.005(2)
C4 0.107(6) 0.046(3) 0.051(3) 0.005(3) 0.019(4) -0.003(4)
C5 0.041(2) 0.024(2) 0.039(2) 0.0012(18) 0.0052(19) -0.0033(17)
C6 0.040(2) 0.0216(19) 0.038(2) -0.0023(17) 0.0004(19) 0.0008(17)
C7 0.058(3) 0.024(2) 0.042(3) 0.0034(18) 0.009(2) -0.004(2)
C8 0.073(5) 0.032(3) 0.041(4) 0.000 0.020(4) 0.000
C9 0.041(3) 0.028(3) 0.033(3) 0.000 0.008(3) 0.000

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O1 2.031(3) . y
Rh1 O3 2.038(3) . y
Rh1 O4 2.040(3) . y
Rh1 O2 2.042(3) . y
Rh1 N1 2.197(4) . y
Rh1 Rh1 2.4137(6) 5_577 y
O1 C1 1.245(6) . ?
O2 C3 1.247(6) . ?
O3 C1 1.243(6) 5_577 ?
O4 C3 1.245(6) 5_577 ?
N1 C5 1.133(6) . ?
C1 O3 1.243(6) 5_577 ?
C1 C2 1.544(8) . ?
C2 F3 1.315(10) . ?
C2 F1 1.327(12) . ?
C2 F2 1.398(12) . ?
C3 O4 1.245(6) 5_577 ?
C3 C4 1.539(8) . ?
C4 F6 1.307(10) . ?
C4 F4 1.359(12) . ?
C4 F5 1.363(11) . ?
C5 C6 1.444(6) . ?
C6 C9 1.384(5) . ?
C6 C7 1.390(7) . ?
C7 C8 1.377(6) . ?
C7 H7 0.9500 . ?
C8 C7 1.377(6) 7_575 ?
C8 H8 0.9500 . ?
C9 C6 1.384(5) 7_575 ?
C9 H9 0.9500 . ?
C10 Cl1 1.72(3) . ?
C10 Cl2 1.75(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10X Cl1X 1.72(3) . ?
C10X Cl2X 1.74(3) . ?
C10X H10C 0.9900 . ?
C10X H10D 0.9900 . ?
C11 C12 1.387(18) . ?
C11 C12 1.387(18) 7_565 ?
C11 H11 0.9500 . ?
C12 C13 1.364(19) . ?
C12 H12 0.9500 . ?
C13 C14 1.35(2) . ?
C13 H13 0.9500 . ?
C14 C13 1.35(2) 7_565 ?
C14 H14 0.9500 . ?
C11X C12X 1.34(2) . ?
C11X C12X 1.34(2) 7_565 ?
C11X H11X 0.9500 . ?
C12X C13X 1.36(2) . ?
C12X H12X 0.9500 . ?
C13X C14X 1.38(2) . ?
C13X H13X 0.9500 . ?
C14X C13X 1.38(2) 7_565 ?
C14X H14X 0.9500 . ?
C15 C16 1.362(12) . ?
C15 C15 1.420(15) 7_565 ?
C15 H15 0.9500 . ?
C16 C17 1.482(13) . ?
C16 H16 0.9500 . ?
C17 C17 1.462(16) 7_565 ?
C17 H17 0.9500 . ?

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
O1 Rh1 O3 175.46(14) . . y
O1 Rh1 O4 89.56(14) . . y
O3 Rh1 O4 91.09(15) . . y
O1 Rh1 O2 90.32(15) . . y
O3 Rh1 O2 88.69(15) . . y
O4 Rh1 O2 175.63(13) . . y
O1 Rh1 N1 91.66(15) . . y
O3 Rh1 N1 92.80(15) . . y
O4 Rh1 N1 92.55(14) . . y
O2 Rh1 N1 91.83(14) . . y
O1 Rh1 Rh1 87.85(10) . 5_577 y
O3 Rh1 Rh1 87.69(10) . 5_577 y
O4 Rh1 Rh1 87.48(9) . 5_577 y
O2 Rh1 Rh1 88.15(10) . 5_577 y
N1 Rh1 Rh1 179.50(12) . 5_577 y
C1 O1 Rh1 117.3(3) . . ?
C3 O2 Rh1 116.7(3) . . ?
C1 O3 Rh1 117.1(3) 5_577 . ?
C3 O4 Rh1 117.6(3) 5_577 . ?
C5 N1 Rh1 175.6(4) . . ?
O3 C1 O1 130.0(5) 5_577 . ?
O3 C1 C2 115.6(5) 5_577 . ?
O1 C1 C2 114.4(5) . . ?
F3 C2 F1 110.2(10) . . ?
F3 C2 F2 111.2(9) . . ?
F1 C2 F2 100.4(10) . . ?
F3 C2 C1 114.6(7) . . ?
F1 C2 C1 112.7(8) . . ?
F2 C2 C1 106.8(7) . . ?
O4 C3 O2 129.9(5) 5_577 . ?
O4 C3 C4 114.7(5) 5_577 . ?
O2 C3 C4 115.4(5) . . ?
F6 C4 F4 109.3(11) . . ?
F6 C4 F5 110.7(10) . . ?
F4 C4 F5 103.8(10) . . ?
F6 C4 C3 113.6(7) . . ?
F4 C4 C3 108.3(8) . . ?
F5 C4 C3 110.6(7) . . ?
N1 C5 C6 179.0(5) . . ?
C9 C6 C7 120.7(4) . . ?
C9 C6 C5 118.8(4) . . ?
C7 C6 C5 120.5(4) . . ?
C8 C7 C6 119.9(5) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 C7 120.0(7) . 7_575 ?
C7 C8 H8 120.0 . . ?
C7 C8 H8 120.0 7_575 . ?
C6 C9 C6 118.7(6) 7_575 . ?
C6 C9 H9 120.6 7_575 . ?
C6 C9 H9 120.6 . . ?
Cl1 C10 Cl2 107.1(19) . . ?
Cl1 C10 H10A 110.3 . . ?
Cl2 C10 H10A 110.3 . . ?
Cl1 C10 H10B 110.3 . . ?
Cl2 C10 H10B 110.3 . . ?
H10A C10 H10B 108.5 . . ?
Cl1X C10X Cl2X 110.4(19) . . ?
Cl1X C10X H10C 109.6 . . ?
Cl2X C10X H10C 109.6 . . ?
Cl1X C10X H10D 109.6 . . ?
Cl2X C10X H10D 109.6 . . ?
H10C C10X H10D 108.1 . . ?
C12 C11 C12 124(3) . 7_565 ?
C12 C11 H11 117.9 . . ?
C12 C11 H11 117.9 7_565 . ?
C13 C12 C11 114.8(16) . . ?
C13 C12 H12 122.6 . . ?
C11 C12 H12 122.6 . . ?
C14 C13 C12 124(2) . . ?
C14 C13 H13 117.9 . . ?
C12 C13 H13 117.9 . . ?
C13 C14 C13 117(3) 7_565 . ?
C13 C14 H14 121.3 7_565 . ?
C13 C14 H14 121.3 . . ?
C12X C11X C12X 116(3) . 7_565 ?
C12X C11X H11X 121.8 . . ?
C12X C11X H11X 121.8 7_565 . ?
C11X C12X C13X 123.7(19) . . ?
C11X C12X H12X 118.1 . . ?
C13X C12X H12X 118.1 . . ?
C12X C13X C14X 119.3(19) . . ?
C12X C13X H13X 120.4 . . ?
C14X C13X H13X 120.4 . . ?
C13X C14X C13X 118(3) 7_565 . ?
C13X C14X H14X 121.1 7_565 . ?
C13X C14X H14X 121.1 . . ?
C16 C15 C15 128.5(7) . 7_565 ?
C16 C15 H15 115.8 . . ?
C15 C15 H15 115.8 7_565 . ?
C15 C16 C17 107.5(11) . . ?
C15 C16 H16 126.2 . . ?
C17 C16 H16 126.2 . . ?
C17 C17 C16 123.9(6) 7_565 . ?
C16 C17 Cl1 110.0(10) . 7_565 ?
C17 C17 H17 118.0 7_565 . ?
C16 C17 H17 118.0 . . ?

_diffrn_measured_fraction_theta_max 0.952
_diffrn_reflns_theta_full        28.32
_diffrn_measured_fraction_theta_full 0.952
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.850
_refine_diff_density_rms         0.122

#===END