# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012
#######################################################################
#
# Cambridge Crystallographic Data Centre
# CCDC
#
#######################################################################
#
# This CIF contains data from an original supplementary publication
# deposited with the CCDC, and may include chemical, crystal,
# experimental, refinement, atomic coordinates,
# anisotropic displacement parameters and molecular geometry data,
# as required by the journal to which it was submitted.
#
# This CIF is provided on the understanding that it is used for bona
# fide research purposes only. It may contain copyright material
# of the CCDC or of third parties, and may not be copied or further
# disseminated in any form, whether machine-readable or not,
# except for the purpose of generating routine backup copies
# on your local computer system.
#
# For further information on the CCDC, data deposition and
# data retrieval see:
# www.ccdc.cam.ac.uk
#
# Bona fide researchers may freely download Mercury and enCIFer
# from this site to visualise CIF-encoded structures and
# to carry out CIF format checking respectively.
#
#######################################################################
data_Rh-pF-phz-dry
_database_code_depnum_ccdc_archive 'CCDC 895508'
#TrackingRef 'CCDC-895508_R2.cif'
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common (Rh2(p-F-PhCO2)4(phz))
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety ?
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C40 H24 F4 N2 O8 Rh2'
_chemical_formula_weight 942.43
_chemical_melting_point ?
_chemical_compound_source ? # for minerals and
# natural products
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Rh Rh -1.0036 1.1392 'International Tables for Crystallography, Vol. C'
C C 0.0033 0.0021 'International Tables for Crystallography, Vol. C'
O O 0.0113 0.0079 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
N N 0.0063 0.0043 'International Tables for Crystallography, Vol. C'
F F 0.0186 0.0133 'International Tables for Crystallography, Vol. C'
#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
_cell_length_a 9.8967(7)
_cell_length_b 10.9360(8)
_cell_length_c 11.3457(7)
_cell_angle_alpha 65.996(5)
_cell_angle_beta 66.173(6)
_cell_angle_gamma 65.291(6)
_cell_volume 977.7(1)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z 1
_cell_measurement_temperature 195(1)
_cell_special_details ?
_exptl_crystal_density_diffrn 1.6006
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 936.00
# 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 ? # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick ? # parallel to
# scattering vector
# in reflection
# The next five fields are character fields that describe the specimen.
_pd_spec_mounting
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode reflection
_pd_spec_shape flat_sheet
_pd_char_particle_morphology ?
_pd_char_colour ?
# 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 ?
_exptl_absorpt_coefficient_mu ?
# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_correction_type ? # include if applicable
_exptl_absorpt_process_details ? # include if applicable
_exptl_absorpt_correction_T_min ? # include if applicable
_exptl_absorpt_correction_T_max ? # include if applicable
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
# 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
; ?
;
_pd_calibration_special_details
# description of the method used
# to calibrate the instrument
; ?
;
_diffrn_ambient_temperature 195(1)
_diffrn_source synchrotron
_diffrn_source_target ?
_diffrn_source_type ?
_diffrn_radiation_type synchrotron
_diffrn_measurement_device_type debye-scherrer
_diffrn_detector 'imaging plate'
_diffrn_detector_type ?
_pd_meas_scan_method step # options are 'step', 'cont',
#' 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details
; ?
;
_diffrn_radiation_wavelength 0.799090
_diffrn_radiation_monochromator 'Si crystal'
# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.
_pd_meas_number_of_points 4701
_pd_meas_2theta_range_min 3.0000
_pd_meas_2theta_range_max 50.0000
_pd_meas_2theta_range_inc 0.0100
# The following three items are used for time-of-flight measurements only.
_pd_instr_dist_src/spec ?
_pd_instr_dist_spec/detc ?
_pd_meas_2theta_fixed ?
#===============================================================================
# 8. 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_calc_method 'Rietveld Refinement'
_pd_proc_ls_profile_function 'split Pearson VII function'
_pd_proc_ls_background_function 'composite background function'
_pd_proc_ls_pref_orient_corr
; ?
;
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and r = 1.0(0)
_pd_proc_ls_prof_R_factor 0.01687
_pd_proc_ls_prof_wR_factor 0.02556
_pd_proc_ls_prof_wR_expected 0.00671
_refine_ls_R_I_factor 0.00966
_refine_ls_R_Fsqd_factor 0.00425
_refine_ls_R_factor_all 0.00427
_refine_special_details
; ?
;
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details 1/y~i~
# The following line must be commented out in the absence of H atoms.
#_refine_ls_hydrogen_treatment ?
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_parameters 91
_refine_ls_number_restraints 0
_refine_ls_number_constraints 26
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all 3.8091
_refine_ls_restrained_S_all ?
# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max 0.0
_refine_ls_shift/su_mean ?
_refine_diff_density_max 0.0
_refine_diff_density_min 0.0
# 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 3.0000
_pd_proc_2theta_range_max 50.0000
_pd_proc_2theta_range_inc 0.0100
_pd_proc_wavelength ?
# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.
_pd_block_diffractogram_id ?
# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions ?
_pd_proc_info_data_reduction ?
# The following items are used to identify the programs used.
_computing_data_collection ?
_computing_cell_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction ?
_computing_structure_solution FOX
_computing_structure_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics 'VESTA (Momma and Izumi, 2008)'
_computing_publication_material ?
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
C1 0.338(6) 0.734(5) 0.066(7) 1 2 i Uiso 0.01475 C
C2 0.246(7) 0.864(5) 0.107(5) 1 2 i Uiso 0.01475 C
C3 0.090(8) 0.900(6) 0.144(6) 1 2 i Uiso 0.01475 C
C4 -0.002(6) 0.023(6) 0.184(6) 1 2 i Uiso 0.01475 C
C5 0.066(6) 0.112(5) 0.186(6) 1 2 i Uiso 0.01475 C
C6 0.222(7) 0.077(6) 0.149(6) 1 2 i Uiso 0.01475 C
C7 0.314(7) 0.953(6) 0.110(6) 1 2 i Uiso 0.01475 C
C8 0.491(7) 0.338(6) 0.243(4) 1 2 i Uiso 0.01475 C
C9 0.475(7) 0.250(5) 0.385(5) 1 2 i Uiso 0.01475 C
C10 0.588(7) 0.217(6) 0.448(6) 1 2 i Uiso 0.01475 C
C11 0.569(6) 0.132(6) 0.582(7) 1 2 i Uiso 0.01475 C
C12 0.442(7) 0.079(4) 0.656(5) 1 2 i Uiso 0.01475 C
C13 0.331(7) 0.116(6) 0.589(6) 1 2 i Uiso 0.01475 C
C14 0.347(7) 0.200(7) 0.455(6) 1 2 i Uiso 0.01475 C
C15 0.020(9) 0.505(6) 0.115(6) 1 2 i Uiso 0.01475 C
C16 0.033(6) 0.513(6) 0.230(6) 1 2 i Uiso 0.01475 C
C17 0.094(7) 0.442(6) 0.676(5) 1 2 i Uiso 0.01475 C
C18 0.241(6) 0.402(6) 0.692(5) 1 2 i Uiso 0.01475 C
C19 0.261(6) 0.405(5) 0.804(6) 1 2 i Uiso 0.01475 C
C20 0.130(8) 0.452(7) 0.904(6) 1 2 i Uiso 0.01475 C
O1 0.265(4) 0.669(4) 0.060(4) 1 2 i Uiso 0.01475 O
O2 0.482(4) 0.701(4) 0.037(4) 1 2 i Uiso 0.01475 O
O3 0.377(4) 0.380(4) 0.200(4) 1 2 i Uiso 0.01475 O
O4 0.599(4) 0.390(4) 0.187(4) 1 2 i Uiso 0.01475 O
F1 -0.021(3) 0.229(2) 0.225(3) 1 2 i Uiso 0.01475 F
F2 0.426(4) -0.006(3) 0.787(3) 1 2 i Uiso 0.01475 F
N1 0.147(5) 0.456(5) 0.017(6) 1 2 i Uiso 0.01475 N
Rh1 0.3827(8) 0.4864(8) 0.006(1) 1 2 i Uiso 0.01226 Rh
H3 0.04489 0.83908 0.1428 1 2 i Uiso 0.01771 H
H4 -0.11177 0.04696 0.21034 1 2 i Uiso 0.01771 H
H6 0.26758 0.13766 0.15062 1 2 i Uiso 0.01771 H
H7 0.4241 0.92925 0.0839 1 2 i Uiso 0.01771 H
H10 0.67548 0.25108 0.39977 1 2 i Uiso 0.01771 H
H11 0.6448 0.10886 0.6256 1 2 i Uiso 0.01771 H
H13 0.2435 0.08197 0.63731 1 2 i Uiso 0.01771 H
H14 0.27146 0.22329 0.41138 1 2 i Uiso 0.01771 H
H16 0.13252 0.48544 0.24194 1 2 i Uiso 0.01771 H
H17 0.08236 0.43865 0.59809 1 2 i Uiso 0.01771 H
H18 0.33169 0.36979 0.62536 1 2 i Uiso 0.01771 H
H19 0.36069 0.37784 0.81564 1 2 i Uiso 0.01771 H
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_geom_special_details ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 C3 1.35(8) . 1_555 ?
C2 C7 1.41(7) . 1_555 ?
C3 C4 1.41(7) . 1_565 ?
C1 O2 1.24(5) . 1_555 ?
C1 O1 1.24(5) . 1_555 ?
C1 C2 1.48(5) . 1_555 ?
C4 C5 1.41(6) . 1_555 ?
C6 C7 1.41(7) . 1_545 ?
C5 F1 1.34(4) . 1_555 ?
C5 C6 1.35(7) . 1_555 ?
O2 Rh1 2.05(4) . 2_665 ?
O1 Rh1 2.05(4) . 1_555 ?
C9 C14 1.40(6) . 1_555 ?
C9 C10 1.41(7) . 1_555 ?
C10 C11 1.41(8) . 1_555 ?
C8 O3 1.24(5) . 1_555 ?
C8 O4 1.24(6) . 1_555 ?
C8 C9 1.48(6) . 1_555 ?
C13 C14 1.41(7) . 1_555 ?
C11 C12 1.41(6) . 1_555 ?
C12 F2 1.38(5) . 1_555 ?
C12 C13 1.41(7) . 1_555 ?
O4 Rh1 2.03(4) . 2_665 ?
O3 Rh1 2.03(4) . 1_555 ?
N1 Rh1 2.43(4) . 1_555 ?
C15 N1 1.38(7) . 1_555 ?
C15 C16 1.40(6) . 1_555 ?
C15 C20 1.44(5) . 2_566 ?
C20 N1 1.38(7) . 1_556 ?
C19 C20 1.40(6) . 1_555 ?
C18 C19 1.38(6) . 1_555 ?
C17 C18 1.40(7) . 1_555 ?
C16 C17 1.34(7) . 2_566 ?
Rh1 Rh1 2.41(1) . 2_665 ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C7 118(5) 1_555 . 1_555 ?
C3 C2 C1 119(5) 1_555 . 1_555 ?
C7 C2 C1 123(5) 1_555 . 1_555 ?
O1 C2 C4 121(4) 1_555 . 1_565 ?
O2 C2 C6 124(3) 1_555 . 1_565 ?
C2 C3 C4 120(6) 1_555 . 1_565 ?
C1 C3 C5 123(3) 1_555 . 1_565 ?
O1 C3 C6 122(3) 1_555 . 1_565 ?
C2 C7 C6 121(6) 1_555 . 1_565 ?
C5 C7 C1 121(3) 1_565 . 1_555 ?
O2 C1 O1 125(4) 1_555 . 1_555 ?
O2 C1 C2 118(5) 1_555 . 1_555 ?
O1 C1 C2 117(5) 1_555 . 1_555 ?
C5 C4 C3 121(6) 1_555 . 1_545 ?
F1 C4 C2 121(3) 1_555 . 1_545 ?
C5 C6 C7 120(7) 1_555 . 1_545 ?
F1 C6 C2 121(3) 1_555 . 1_545 ?
F1 C5 C6 120(6) 1_555 . 1_555 ?
F1 C5 C4 121(5) 1_555 . 1_555 ?
C6 C5 C4 119(5) 1_555 . 1_555 ?
C14 C9 C10 120(5) 1_555 . 1_555 ?
C14 C9 C8 119(6) 1_555 . 1_555 ?
C10 C9 C8 121(6) 1_555 . 1_555 ?
O3 C9 C13 121(4) 1_555 . 1_555 ?
O4 C9 C11 123(4) 1_555 . 1_555 ?
C9 C14 C13 120(5) 1_555 . 1_555 ?
C12 C14 C8 122(3) 1_555 . 1_555 ?
O3 C14 C11 118(3) 1_555 . 1_555 ?
C11 C10 C9 119(6) 1_555 . 1_555 ?
C12 C10 C8 120(3) 1_555 . 1_555 ?
O4 C10 C13 117(3) 1_555 . 1_555 ?
O3 C8 O4 123(4) 1_555 . 1_555 ?
O3 C8 C9 117(6) 1_555 . 1_555 ?
O4 C8 C9 118(5) 1_555 . 1_555 ?
C14 C13 C12 122(6) 1_555 . 1_555 ?
C9 C13 F2 121(3) 1_555 . 1_555 ?
C10 C11 C12 123(6) 1_555 . 1_555 ?
C9 C11 F2 121(3) 1_555 . 1_555 ?
F2 C12 C13 121(6) 1_555 . 1_555 ?
F2 C12 C11 122(6) 1_555 . 1_555 ?
C13 C12 C11 117(4) 1_555 . 1_555 ?
C15 N1 C20 121(4) 1_555 . 1_554 ?
C19 N1 C20 119(3) 1_554 . 2_566 ?
C16 N1 C15 120(3) 1_555 . 2_565 ?
N1 C15 C16 123(7) 1_555 . 1_555 ?
N1 C15 C20 117(6) 1_555 . 2_566 ?
C16 C15 C20 120(7) 1_555 . 2_566 ?
C17 C15 N1 119(4) 2_566 . 2_565 ?
C20 C15 C19 118(5) 1_554 . 2_566 ?
C18 C15 C15 118(5) 2_566 . 2_565 ?
N1 C20 C19 120(7) 1_556 . 1_555 ?
N1 C20 C15 122(6) 1_556 . 2_566 ?
C19 C20 C15 118(7) 1_555 . 2_566 ?
C18 C20 N1 119(4) 1_555 . 2_566 ?
C15 C20 C16 122(5) 1_556 . 2_566 ?
C18 C19 C20 119(6) 1_555 . 1_555 ?
N1 C19 C17 120(3) 1_556 . 1_555 ?
C19 C18 C17 122(5) 1_555 . 1_555 ?
C16 C17 C18 120(6) 2_566 . 1_555 ?
C17 C16 C15 120(6) 2_566 . 1_555 ?
C18 C16 N1 118(3) 2_566 . 1_555 ?
data_Rh-pF-phz_2
_database_code_depnum_ccdc_archive 'CCDC 895509'
#TrackingRef 'Rh-pF-phz.cif'
#==============================================================================
# CHEMICAL DATA
_chemical_formula_sum 'C52 H34 F4 N4 O12 Rh2'
_chemical_formula_moiety 'C52 H34 F4 N4 O12 Rh2'
_chemical_formula_weight 1188.66
_chemical_melting_point ?
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a 9.977(3)
_cell_length_b 11.801(4)
_cell_length_c 20.095(6)
_cell_angle_alpha 90.0000
_cell_angle_beta 90.418(4)
_cell_angle_gamma 90.0000
_cell_volume 2365.9(12)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 7409
_cell_measurement_theta_min 3.35
_cell_measurement_theta_max 27.49
_cell_measurement_temperature 123
#------------------------------------------------------------------------------
_exptl_crystal_description platelet
_exptl_crystal_colour red-brown
_exptl_crystal_size_max 0.300
_exptl_crystal_size_mid 0.100
_exptl_crystal_size_min 0.010
_exptl_crystal_density_diffrn 1.668
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1192.00
_exptl_absorpt_coefficient_mu 0.782
_exptl_absorpt_correction_type none
#==============================================================================
# EXPERIMENTAL DATA
_diffrn_ambient_temperature 123
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71070
_diffrn_measurement_device_type 'Rigaku Mercury70'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 7.314
_diffrn_reflns_number 21851
_diffrn_reflns_av_R_equivalents 0.0807
_diffrn_reflns_theta_max 25.00
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 23
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_decay_% ?
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
Refinement was performed using all reflections. The weighted
R-factor (wR) and goodness of fit (S) are based on F^2^.
R-factor (gt) are based on F. The threshold expression of
F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt).
;
_reflns_number_total 4150
_reflns_number_gt 3194
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt 0.0818
_refine_ls_wR_factor_ref 0.1645
_refine_ls_number_restraints 0
_refine_ls_hydrogen_treatment constr
_refine_ls_number_reflns 4143
_refine_ls_number_parameters 334
_refine_ls_goodness_of_fit_ref 1.127
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0227P)^2^+21.6482P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_diff_density_max 0.960
_refine_diff_density_min -1.330
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Rh Rh -1.1178 0.9187
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS
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 0.12092(5) 0.50190(6) 0.49952(3) 0.0320(3) Uani 1.0 4 d . . .
F1 F -0.0131(10) 0.6130(7) 0.1003(3) 0.114(3) Uani 1.0 4 d . . .
F2 F 0.0119(10) -0.1620(5) 0.3793(4) 0.109(3) Uani 1.0 4 d . . .
O1 O 0.1089(5) 0.5576(5) 0.4042(3) 0.0361(13) Uani 1.0 4 d . . .
O2 O -0.1167(5) 0.5557(5) 0.4049(3) 0.0362(13) Uani 1.0 4 d . . .
O3 O 0.1152(5) 0.3384(5) 0.4688(3) 0.0342(13) Uani 1.0 4 d . . .
O4 O -0.1107(5) 0.3348(5) 0.4696(3) 0.0377(13) Uani 1.0 4 d . . .
O5 O 0.1099(8) 0.2996(7) 0.2887(4) 0.076(3) Uani 1.0 4 d . . .
O6 O -0.1086(8) 0.2983(8) 0.2878(4) 0.079(3) Uani 1.0 4 d . . .
N1 N 0.3583(5) 0.5005(6) 0.4998(3) 0.0218(12) Uani 1.0 4 d . . .
N2 N 0.0007(10) 0.2932(7) 0.2595(5) 0.059(3) Uani 1.0 4 d . . .
C1 C -0.0053(9) 0.5661(7) 0.3771(5) 0.040(2) Uani 1.0 4 d . . .
C2 C -0.0086(10) 0.5844(8) 0.3029(5) 0.046(3) Uani 1.0 4 d . . .
C3 C 0.1123(11) 0.5921(9) 0.2699(5) 0.058(3) Uani 1.0 4 d . . .
C4 C 0.1096(15) 0.6017(11) 0.1997(6) 0.081(4) Uani 1.0 4 d . . .
C5 C -0.0148(18) 0.6038(11) 0.1694(6) 0.083(4) Uani 1.0 4 d . . .
C6 C -0.1327(14) 0.5961(11) 0.2005(6) 0.074(4) Uani 1.0 4 d . . .
C7 C -0.1290(11) 0.5847(9) 0.2687(5) 0.057(3) Uani 1.0 4 d . . .
C8 C 0.0036(8) 0.2903(7) 0.4606(4) 0.0348(19) Uani 1.0 4 d . . .
C9 C 0.0058(9) 0.1697(8) 0.4381(4) 0.039(2) Uani 1.0 4 d . . .
C10 C -0.1114(11) 0.1105(9) 0.4319(5) 0.059(3) Uani 1.0 4 d . . .
C11 C -0.1094(14) -0.0059(10) 0.4125(6) 0.072(4) Uani 1.0 4 d . . .
C12 C 0.0115(15) -0.0518(9) 0.3992(6) 0.073(4) Uani 1.0 4 d . . .
C13 C 0.1278(13) 0.0063(10) 0.4062(6) 0.073(4) Uani 1.0 4 d . . .
C14 C 0.1252(11) 0.1166(8) 0.4262(5) 0.058(3) Uani 1.0 4 d . . .
C15 C 0.4268(7) 0.4641(7) 0.4461(4) 0.0302(18) Uani 1.0 4 d . . .
C16 C 0.3583(8) 0.4244(8) 0.3889(4) 0.038(2) Uani 1.0 4 d . . .
C17 C 0.4285(8) 0.3888(8) 0.3340(5) 0.041(2) Uani 1.0 4 d . . .
C18 C 0.5684(8) 0.3850(8) 0.3352(5) 0.041(2) Uani 1.0 4 d . . .
C19 C 0.6381(8) 0.4182(8) 0.3903(5) 0.039(2) Uani 1.0 4 d . . .
C20 C 0.5722(7) 0.4625(6) 0.4481(4) 0.0280(17) Uani 1.0 4 d . . .
C21 C -0.0004(9) 0.2807(7) 0.1864(5) 0.042(2) Uani 1.0 4 d . . .
C22 C -0.1231(9) 0.2740(7) 0.1537(5) 0.046(3) Uani 1.0 4 d . . .
C23 C -0.1213(11) 0.2628(8) 0.0854(6) 0.057(3) Uani 1.0 4 d . . .
C24 C -0.0028(13) 0.2595(8) 0.0514(5) 0.060(3) Uani 1.0 4 d . . .
C25 C 0.1171(11) 0.2648(8) 0.0857(6) 0.055(3) Uani 1.0 4 d . . .
C26 C 0.1202(9) 0.2757(8) 0.1532(5) 0.050(3) Uani 1.0 4 d . . .
H3 H 0.1948 0.5911 0.2937 0.0701 Uiso 1.0 4 calc R . .
H4 H 0.1898 0.6064 0.1746 0.0969 Uiso 1.0 4 calc R . .
H6 H -0.2152 0.5983 0.1766 0.0883 Uiso 1.0 4 calc R . .
H7 H -0.2104 0.5770 0.2925 0.0683 Uiso 1.0 4 calc R . .
H10 H -0.1944 0.1468 0.4407 0.0707 Uiso 1.0 4 calc R . .
H11 H -0.1895 -0.0490 0.4090 0.0859 Uiso 1.0 4 calc R . .
H13 H 0.2109 -0.0297 0.3971 0.0873 Uiso 1.0 4 calc R . .
H14 H 0.2068 0.1569 0.4320 0.0702 Uiso 1.0 4 calc R . .
H16 H 0.2631 0.4224 0.3882 0.0461 Uiso 1.0 4 calc R . .
H17 H 0.3813 0.3665 0.2949 0.0497 Uiso 1.0 4 calc R . .
H18 H 0.6154 0.3590 0.2972 0.0497 Uiso 1.0 4 calc R . .
H19 H 0.7331 0.4120 0.3905 0.0473 Uiso 1.0 4 calc R . .
H22 H -0.2051 0.2770 0.1774 0.0549 Uiso 1.0 4 calc R . .
H23 H -0.2035 0.2572 0.0615 0.0683 Uiso 1.0 4 calc R . .
H24 H -0.0034 0.2535 0.0043 0.0720 Uiso 1.0 4 calc R . .
H25 H 0.1989 0.2608 0.0619 0.0657 Uiso 1.0 4 calc R . .
H26 H 0.2030 0.2797 0.1767 0.0604 Uiso 1.0 4 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Rh1 0.0204(4) 0.0394(4) 0.0362(4) 0.0003(3) 0.0009(3) -0.0070(3)
F1 0.193(9) 0.112(7) 0.037(4) 0.012(6) 0.003(5) 0.009(4)
F2 0.179(8) 0.028(4) 0.122(7) 0.001(5) 0.011(6) -0.016(4)
O1 0.031(3) 0.040(4) 0.037(4) -0.005(3) 0.001(3) -0.003(3)
O2 0.029(3) 0.048(4) 0.032(3) 0.001(3) -0.002(3) -0.006(3)
O3 0.028(3) 0.037(4) 0.037(4) -0.002(3) 0.001(3) -0.009(3)
O4 0.029(3) 0.035(4) 0.049(4) -0.000(3) 0.001(3) -0.010(3)
O5 0.078(6) 0.078(6) 0.071(5) -0.017(5) -0.023(5) 0.013(5)
O6 0.078(6) 0.098(7) 0.060(5) 0.003(5) 0.019(4) 0.010(5)
N1 0.007(3) 0.034(4) 0.024(3) 0.002(3) -0.005(2) -0.004(3)
N2 0.066(6) 0.046(5) 0.066(6) -0.007(5) 0.000(5) 0.006(5)
C1 0.046(6) 0.025(5) 0.048(6) -0.004(4) -0.004(4) -0.014(4)
C2 0.056(6) 0.038(5) 0.042(6) 0.003(5) 0.009(5) -0.008(4)
C3 0.074(7) 0.052(7) 0.049(6) -0.014(6) 0.003(5) 0.008(5)
C4 0.119(11) 0.070(8) 0.054(8) -0.013(8) 0.030(8) -0.003(6)
C5 0.145(14) 0.063(8) 0.041(7) 0.010(9) -0.013(8) 0.008(6)
C6 0.089(9) 0.086(9) 0.046(7) 0.019(8) 0.001(6) 0.010(6)
C7 0.080(8) 0.048(6) 0.042(6) 0.012(6) -0.011(5) 0.002(5)
C8 0.037(5) 0.041(5) 0.026(5) 0.004(4) 0.001(4) 0.006(4)
C9 0.046(5) 0.041(5) 0.031(5) -0.002(5) 0.003(4) -0.005(4)
C10 0.066(7) 0.050(6) 0.062(7) -0.003(6) 0.015(5) -0.012(5)
C11 0.104(10) 0.044(6) 0.067(8) -0.020(7) 0.015(7) -0.012(6)
C12 0.127(11) 0.026(6) 0.065(8) 0.001(7) 0.012(7) -0.003(5)
C13 0.086(9) 0.041(6) 0.091(9) 0.017(7) -0.010(7) -0.017(6)
C14 0.061(7) 0.039(6) 0.075(8) 0.008(5) -0.009(6) -0.015(5)
C15 0.021(4) 0.037(5) 0.032(5) 0.009(4) 0.012(3) -0.004(4)
C16 0.032(5) 0.049(6) 0.034(5) -0.006(4) 0.004(4) -0.013(4)
C17 0.030(5) 0.050(6) 0.044(6) -0.002(4) -0.004(4) -0.017(5)
C18 0.036(5) 0.046(6) 0.042(5) 0.002(4) 0.003(4) -0.014(4)
C19 0.023(4) 0.045(5) 0.050(6) 0.003(4) 0.002(4) -0.012(4)
C20 0.023(4) 0.021(4) 0.040(5) -0.006(3) 0.003(3) -0.004(4)
C21 0.048(6) 0.030(5) 0.047(6) -0.001(4) -0.002(4) -0.001(4)
C22 0.038(5) 0.032(5) 0.067(7) 0.006(4) -0.004(5) -0.002(5)
C23 0.063(7) 0.034(6) 0.074(8) 0.003(5) -0.023(6) -0.008(5)
C24 0.092(9) 0.041(6) 0.047(6) -0.001(6) -0.008(6) -0.005(5)
C25 0.061(7) 0.039(6) 0.064(7) 0.001(5) 0.025(6) -0.010(5)
C26 0.035(5) 0.042(6) 0.073(8) -0.003(5) -0.002(5) 0.007(5)
#==============================================================================
_computing_data_collection 'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement CrystalClear
_computing_data_reduction CrystalClear
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_molecular_graphics 'CrystalStructure 4.0'
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Rh1 Rh1 2.4134(10) yes . 3_566
Rh1 O1 2.027(6) yes . .
Rh1 O2 2.038(6) yes . 3_566
Rh1 O3 2.027(6) yes . .
Rh1 O4 2.027(6) yes . 3_566
Rh1 N1 2.368(5) yes . .
F1 C5 1.393(13) yes . .
F2 C12 1.360(12) yes . .
O1 C1 1.264(10) yes . .
O2 C1 1.253(10) yes . .
O3 C8 1.259(10) yes . .
O4 C8 1.269(10) yes . .
O5 N2 1.237(12) yes . .
O6 N2 1.236(13) yes . .
N1 C15 1.351(9) yes . .
N1 C20 1.326(9) yes . 3_666
N2 C21 1.475(13) yes . .
C1 C2 1.505(13) yes . .
C2 C3 1.384(14) yes . .
C2 C7 1.379(14) yes . .
C3 C4 1.415(15) yes . .
C4 C5 1.38(3) yes . .
C5 C6 1.34(2) yes . .
C6 C7 1.377(15) yes . .
C8 C9 1.493(12) yes . .
C9 C10 1.367(14) yes . .
C9 C14 1.369(14) yes . .
C10 C11 1.427(15) yes . .
C11 C12 1.35(2) yes . .
C12 C13 1.354(19) yes . .
C13 C14 1.362(15) yes . .
C15 C16 1.414(11) yes . .
C15 C20 1.451(10) yes . .
C16 C17 1.376(12) yes . .
C17 C18 1.396(11) yes . .
C18 C19 1.361(12) yes . .
C19 C20 1.438(11) yes . .
C21 C22 1.388(13) yes . .
C21 C26 1.381(13) yes . .
C22 C23 1.380(15) yes . .
C23 C24 1.370(16) yes . .
C24 C25 1.377(16) yes . .
C25 C26 1.363(15) yes . .
C3 H3 0.950 no . .
C4 H4 0.950 no . .
C6 H6 0.950 no . .
C7 H7 0.950 no . .
C10 H10 0.950 no . .
C11 H11 0.950 no . .
C13 H13 0.950 no . .
C14 H14 0.950 no . .
C16 H16 0.950 no . .
C17 H17 0.950 no . .
C18 H18 0.950 no . .
C19 H19 0.950 no . .
C22 H22 0.950 no . .
C23 H23 0.950 no . .
C24 H24 0.950 no . .
C25 H25 0.950 no . .
C26 H26 0.950 no . .
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
Rh1 Rh1 O1 87.79(15) yes 3_566 . .
Rh1 Rh1 O2 87.62(15) yes 3_566 . 3_566
Rh1 Rh1 O3 87.63(14) yes 3_566 . .
Rh1 Rh1 O4 87.85(15) yes 3_566 . 3_566
Rh1 Rh1 N1 178.42(15) yes 3_566 . .
O1 Rh1 O2 175.4(2) yes . . 3_566
O1 Rh1 O3 91.1(3) yes . . .
O1 Rh1 O4 88.7(3) yes . . 3_566
O1 Rh1 N1 93.2(2) yes . . .
O2 Rh1 O3 88.2(3) yes 3_566 . .
O2 Rh1 O4 91.6(3) yes 3_566 . 3_566
O2 Rh1 N1 91.4(2) yes 3_566 . .
O3 Rh1 O4 175.5(2) yes . . 3_566
O3 Rh1 N1 91.1(2) yes . . .
O4 Rh1 N1 93.4(2) yes 3_566 . .
Rh1 O1 C1 118.7(6) yes . . .
Rh1 O2 C1 118.6(5) yes 3_566 . .
Rh1 O3 C8 119.5(5) yes . . .
Rh1 O4 C8 119.0(5) yes 3_566 . .
Rh1 N1 C15 120.8(5) yes . . .
Rh1 N1 C20 121.1(5) yes . . 3_666
C15 N1 C20 118.0(6) yes . . 3_666
O5 N2 O6 123.7(9) yes . . .
O5 N2 C21 118.6(9) yes . . .
O6 N2 C21 117.6(9) yes . . .
O1 C1 O2 126.8(8) yes . . .
O1 C1 C2 116.9(8) yes . . .
O2 C1 C2 116.3(8) yes . . .
C1 C2 C3 118.1(9) yes . . .
C1 C2 C7 120.4(9) yes . . .
C3 C2 C7 121.3(9) yes . . .
C2 C3 C4 118.3(11) yes . . .
C3 C4 C5 116.9(12) yes . . .
F1 C5 C4 115.1(13) yes . . .
F1 C5 C6 119.2(13) yes . . .
C4 C5 C6 125.7(11) yes . . .
C5 C6 C7 116.9(12) yes . . .
C2 C7 C6 120.9(11) yes . . .
O3 C8 O4 126.0(8) yes . . .
O3 C8 C9 117.0(7) yes . . .
O4 C8 C9 116.9(7) yes . . .
C8 C9 C10 120.0(8) yes . . .
C8 C9 C14 120.3(8) yes . . .
C10 C9 C14 119.6(9) yes . . .
C9 C10 C11 120.2(10) yes . . .
C10 C11 C12 117.1(11) yes . . .
F2 C12 C11 116.5(12) yes . . .
F2 C12 C13 120.7(12) yes . . .
C11 C12 C13 122.8(10) yes . . .
C12 C13 C14 119.7(11) yes . . .
C9 C14 C13 120.6(10) yes . . .
N1 C15 C16 120.6(7) yes . . .
N1 C15 C20 119.6(7) yes . . .
C16 C15 C20 119.8(7) yes . . .
C15 C16 C17 120.4(7) yes . . .
C16 C17 C18 120.7(8) yes . . .
C17 C18 C19 120.7(8) yes . . .
C18 C19 C20 121.9(7) yes . . .
N1 C20 C15 122.4(7) yes 3_666 . .
N1 C20 C19 121.2(7) yes 3_666 . .
C15 C20 C19 116.4(7) yes . . .
N2 C21 C22 118.5(8) yes . . .
N2 C21 C26 119.1(8) yes . . .
C22 C21 C26 122.4(9) yes . . .
C21 C22 C23 117.3(9) yes . . .
C22 C23 C24 121.1(10) yes . . .
C23 C24 C25 119.9(10) yes . . .
C24 C25 C26 121.0(10) yes . . .
C21 C26 C25 118.2(9) yes . . .
C2 C3 H3 120.867 no . . .
C4 C3 H3 120.872 no . . .
C3 C4 H4 121.571 no . . .
C5 C4 H4 121.558 no . . .
C5 C6 H6 121.533 no . . .
C7 C6 H6 121.523 no . . .
C2 C7 H7 119.537 no . . .
C6 C7 H7 119.535 no . . .
C9 C10 H10 119.908 no . . .
C11 C10 H10 119.905 no . . .
C10 C11 H11 121.472 no . . .
C12 C11 H11 121.464 no . . .
C12 C13 H13 120.143 no . . .
C14 C13 H13 120.147 no . . .
C9 C14 H14 119.718 no . . .
C13 C14 H14 119.720 no . . .
C15 C16 H16 119.790 no . . .
C17 C16 H16 119.781 no . . .
C16 C17 H17 119.650 no . . .
C18 C17 H17 119.643 no . . .
C17 C18 H18 119.675 no . . .
C19 C18 H18 119.672 no . . .
C18 C19 H19 119.073 no . . .
C20 C19 H19 119.058 no . . .
C21 C22 H22 121.347 no . . .
C23 C22 H22 121.351 no . . .
C22 C23 H23 119.443 no . . .
C24 C23 H23 119.431 no . . .
C23 C24 H24 120.035 no . . .
C25 C24 H24 120.037 no . . .
C24 C25 H25 119.504 no . . .
C26 C25 H25 119.510 no . . .
C21 C26 H26 120.908 no . . .
C25 C26 H26 120.892 no . . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
Rh1 C16 3.386(8) no . .
Rh1 C19 3.390(8) no . 3_666
F1 C7 3.600(12) no . .
F2 C14 3.600(12) no . .
O1 C3 2.731(11) no . .
O1 C8 3.515(10) no . .
O1 C8 3.451(10) no . 3_566
O1 C15 3.457(9) no . .
O1 C16 2.960(10) no . .
O2 C3 3.585(12) no . .
O2 C7 2.760(11) no . .
O2 C8 3.533(10) no . .
O2 C8 3.441(10) no . 3_566
O3 C1 3.469(10) no . .
O3 C1 3.481(10) no . 3_566
O3 C10 3.587(12) no . .
O3 C14 2.756(11) no . .
O3 C15 3.478(9) no . .
O3 C16 3.090(10) no . .
O4 C1 3.471(10) no . .
O4 C1 3.485(11) no . 3_566
O4 C10 2.754(12) no . .
O4 C14 3.600(12) no . .
O5 C22 3.572(12) no . .
O5 C26 2.741(13) no . .
O6 C22 2.713(13) no . .
O6 C26 3.563(13) no . .
N1 N1 2.828(7) no . 3_666
C2 C5 2.693(15) no . .
C3 C6 2.805(17) no . .
C4 C7 2.770(18) no . .
C9 C12 2.730(13) no . .
C10 C13 2.738(16) no . .
C11 C14 2.762(17) no . .
C15 C15 2.738(11) no . 3_666
C15 C18 2.807(12) no . .
C16 C19 2.793(11) no . .
C16 C20 3.600(11) no . 3_666
C17 C20 2.832(11) no . .
C20 C20 2.692(11) no . 3_666
C21 C24 2.725(14) no . .
C22 C25 2.770(14) no . .
C23 C26 2.762(14) no . .
F1 C18 3.507(12) no . 2_555
F1 C24 3.404(12) no . 3_565
F2 O1 3.483(9) no . 1_545
F2 C1 3.213(10) no . 1_545
F2 C2 3.368(11) no . 1_545
F2 C8 3.561(11) no . 3_556
O1 F2 3.483(9) no . 1_565
O2 C19 2.948(10) no . 1_455
O2 C20 3.412(9) no . 1_455
O2 C23 3.586(12) no . 2_455
O4 C19 3.120(10) no . 1_455
O4 C20 3.529(9) no . 1_455
O5 C2 3.575(12) no . .
O5 C3 3.473(13) no . .
O5 C9 3.533(12) no . .
O5 C14 3.510(13) no . .
O5 C16 3.505(12) no . .
O5 C17 3.464(12) no . .
O6 C2 3.533(13) no . .
O6 C6 3.524(16) no . 2_445
O6 C7 3.408(13) no . .
O6 C9 3.559(12) no . .
O6 C18 3.518(12) no . 1_455
O6 C19 3.564(12) no . 1_455
N1 C23 3.557(12) no . 4_555
N1 C24 3.535(12) no . 2_555
N1 C24 3.519(12) no . 4_555
N1 C25 3.569(12) no . 2_555
N2 C2 3.548(12) no . .
C1 F2 3.213(10) no . 1_565
C2 F2 3.368(11) no . 1_565
C2 O5 3.575(12) no . .
C2 O6 3.533(13) no . .
C2 N2 3.548(12) no . .
C3 O5 3.473(13) no . .
C4 C13 3.569(19) no . 2_555
C4 C17 3.476(15) no . 2_555
C5 C17 3.472(16) no . 2_555
C5 C18 3.363(15) no . 2_555
C6 O6 3.524(16) no . 2_455
C6 C18 3.544(15) no . 2_555
C7 O6 3.408(13) no . .
C8 F2 3.561(11) no . 3_556
C9 O5 3.533(12) no . .
C9 O6 3.559(12) no . .
C9 C12 3.560(14) no . 3_556
C10 C12 3.597(16) no . 3_556
C10 C13 3.538(16) no . 3_556
C11 C14 3.499(15) no . 3_556
C12 C9 3.560(14) no . 3_556
C12 C10 3.597(16) no . 3_556
C13 C4 3.569(19) no . 2_545
C13 C10 3.538(16) no . 3_556
C14 O5 3.510(13) no . .
C14 C11 3.499(15) no . 3_556
C15 C24 3.568(13) no . 2_555
C15 C24 3.450(13) no . 4_555
C16 O5 3.505(12) no . .
C17 O5 3.464(12) no . .
C17 C4 3.476(15) no . 2_545
C17 C5 3.472(16) no . 2_545
C18 F1 3.507(12) no . 2_545
C18 O6 3.518(12) no . 1_655
C18 C5 3.363(15) no . 2_545
C18 C6 3.544(15) no . 2_545
C19 O2 2.948(10) no . 1_655
C19 O4 3.120(10) no . 1_655
C19 O6 3.564(12) no . 1_655
C20 O2 3.412(9) no . 1_655
C20 O4 3.529(9) no . 1_655
C20 C24 3.572(12) no . 2_555
C20 C24 3.428(13) no . 4_555
C23 O2 3.586(12) no . 2_445
C23 N1 3.557(12) no . 4_454
C24 F1 3.404(12) no . 3_565
C24 N1 3.535(12) no . 2_545
C24 N1 3.519(12) no . 4_454
C24 C15 3.568(13) no . 2_545
C24 C15 3.450(13) no . 4_454
C24 C20 3.572(12) no . 2_545
C24 C20 3.428(13) no . 4_454
C25 N1 3.569(12) no . 2_545
Rh1 H16 2.8175 no . .
Rh1 H19 2.8265 no . 3_666
F1 H4 2.5082 no . .
F1 H6 2.5482 no . .
F2 H11 2.4880 no . .
F2 H13 2.5497 no . .
O1 H3 2.4190 no . .
O1 H16 2.2410 no . .
O2 H7 2.4508 no . .
O3 H14 2.4454 no . .
O3 H16 2.4110 no . .
O4 H10 2.4399 no . .
O5 H26 2.4527 no . .
O6 H22 2.4247 no . .
N1 H16 2.5964 no . .
N1 H19 2.6052 no . 3_666
N2 H22 2.6302 no . .
N2 H26 2.6295 no . .
C1 H3 2.6324 no . .
C1 H7 2.6529 no . .
C1 H16 3.1766 no . .
C2 H4 3.2722 no . .
C2 H6 3.2620 no . .
C3 H7 3.2590 no . .
C3 H16 3.4473 no . .
C4 H6 3.2704 no . .
C5 H3 3.2494 no . .
C5 H7 3.1778 no . .
C6 H4 3.2652 no . .
C7 H3 3.2666 no . .
C8 H10 2.6304 no . .
C8 H14 2.6337 no . .
C8 H16 3.3614 no . .
C9 H11 3.2839 no . .
C9 H13 3.2292 no . .
C10 H14 3.2219 no . .
C11 H13 3.2249 no . .
C12 H10 3.2303 no . .
C12 H14 3.2061 no . .
C13 H11 3.2334 no . .
C14 H10 3.2235 no . .
C15 H17 3.2775 no . .
C15 H19 3.3178 no . .
C16 H3 3.1839 no . .
C16 H18 3.2617 no . .
C17 H3 3.4297 no . .
C17 H19 3.2476 no . .
C18 H16 3.2646 no . .
C19 H17 3.2462 no . .
C20 H16 3.3360 no . .
C20 H18 3.3011 no . .
C21 H23 3.2267 no . .
C21 H25 3.2167 no . .
C22 H24 3.2494 no . .
C22 H26 3.2830 no . .
C23 H25 3.2325 no . .
C24 H22 3.2560 no . .
C24 H26 3.2457 no . .
C25 H23 3.2331 no . .
C26 H22 3.2849 no . .
C26 H24 3.2385 no . .
H3 H4 2.3996 no . .
H3 H16 2.8318 no . .
H3 H17 3.2380 no . .
H6 H7 2.3424 no . .
H10 H11 2.3970 no . .
H13 H14 2.3106 no . .
H14 H16 3.3033 no . .
H16 H17 2.3189 no . .
H17 H18 2.3367 no . .
H18 H19 2.2928 no . .
H22 H23 2.3408 no . .
H23 H24 2.3123 no . .
H24 H25 2.3207 no . .
H25 H26 2.3185 no . .
F1 H10 3.0519 no . 2_455
F1 H11 3.5340 no . 2_455
F1 H13 3.4534 no . 2_555
F1 H14 3.1710 no . 2_555
F1 H24 2.6321 no . 3_565
F2 H22 3.3372 no . 2_445
F2 H23 3.4411 no . 2_445
F2 H25 3.2411 no . 2_545
F2 H26 3.1427 no . 2_545
O1 H25 3.1427 no . 2_555
O2 H19 2.2804 no . 1_455
O2 H22 3.5609 no . 2_455
O2 H23 3.0580 no . 2_455
O3 H23 2.8230 no . 4_555
O4 H19 2.3981 no . 1_455
O4 H25 2.8929 no . 4_455
O5 H3 3.5439 no . .
O5 H3 3.5555 no . 2_545
O5 H4 3.1170 no . 2_545
O5 H14 3.4676 no . .
O5 H16 2.8964 no . .
O5 H17 2.8228 no . .
O6 H6 3.0311 no . 2_445
O6 H7 3.4441 no . .
O6 H7 3.5554 no . 2_445
O6 H18 2.8527 no . 1_455
O6 H19 2.9328 no . 1_455
N1 H23 3.3442 no . 4_555
N1 H24 3.3194 no . 2_555
N1 H24 3.3004 no . 4_555
N1 H25 3.3596 no . 2_555
C1 H19 3.1944 no . 1_455
C3 H17 3.4908 no . 2_555
C3 H26 3.0693 no . 2_555
C4 H13 3.0736 no . 2_555
C4 H14 3.2949 no . 2_555
C4 H17 3.1288 no . 2_555
C5 H17 3.4476 no . 2_555
C5 H18 3.2463 no . 2_555
C6 H10 3.3626 no . 2_455
C6 H11 3.2967 no . 2_455
C6 H18 3.1080 no . 2_555
C7 H18 3.5001 no . 2_555
C7 H19 3.4777 no . 1_455
C7 H22 3.0146 no . 2_455
C8 H19 3.3576 no . 1_455
C8 H23 3.5890 no . 4_555
C10 H6 2.7779 no . 2_445
C10 H25 3.5744 no . 4_455
C11 H6 2.7811 no . 2_445
C11 H23 3.4040 no . 2_445
C13 H4 2.7177 no . 2_545
C13 H25 3.4316 no . 2_545
C13 H26 3.5796 no . 2_545
C14 H4 2.7543 no . 2_545
C14 H11 3.4604 no . 3_556
C14 H23 3.5306 no . 4_555
C15 H24 2.9031 no . 4_555
C16 H24 3.4122 no . 4_555
C17 H4 3.5395 no . 2_545
C18 H7 3.2817 no . 1_655
C19 H7 3.1146 no . 1_655
C19 H24 3.3752 no . 4_555
C20 H24 2.8896 no . 4_555
C22 H7 3.0585 no . 2_445
C22 H11 3.0684 no . 2_455
C23 H11 2.9178 no . 2_455
C25 H13 2.9897 no . 2_555
C26 H3 3.0432 no . 2_545
C26 H13 3.0271 no . 2_555
H3 O5 3.5439 no . .
H3 O5 3.5555 no . 2_555
H3 C26 3.0432 no . 2_555
H3 H26 2.5176 no . 2_555
H4 O5 3.1170 no . 2_555
H4 C13 2.7177 no . 2_555
H4 C14 2.7543 no . 2_555
H4 C17 3.5395 no . 2_555
H4 H13 2.3791 no . 2_555
H4 H14 2.4587 no . 2_555
H4 H17 3.2110 no . 2_555
H6 O6 3.0311 no . 2_455
H6 C10 2.7779 no . 2_455
H6 C11 2.7811 no . 2_455
H6 H10 2.5813 no . 2_455
H6 H11 2.6205 no . 2_455
H6 H18 3.2752 no . 2_555
H7 O6 3.4441 no . .
H7 O6 3.5554 no . 2_455
H7 C18 3.2817 no . 1_455
H7 C19 3.1146 no . 1_455
H7 C22 3.0585 no . 2_455
H7 H18 3.1071 no . 1_455
H7 H19 2.8302 no . 1_455
H7 H22 2.5791 no . 2_455
H10 F1 3.0519 no . 2_445
H10 C6 3.3626 no . 2_445
H10 H6 2.5813 no . 2_445
H10 H13 3.5452 no . 3_556
H10 H19 3.3649 no . 1_455
H10 H24 3.5467 no . 4_455
H10 H25 2.8793 no . 4_455
H11 F1 3.5340 no . 2_445
H11 C6 3.2967 no . 2_445
H11 C14 3.4604 no . 3_556
H11 C22 3.0684 no . 2_445
H11 C23 2.9178 no . 2_445
H11 H6 2.6205 no . 2_445
H11 H14 3.4436 no . 3_556
H11 H22 2.8835 no . 2_445
H11 H23 2.5932 no . 2_445
H13 F1 3.4534 no . 2_545
H13 C4 3.0736 no . 2_545
H13 C25 2.9897 no . 2_545
H13 C26 3.0271 no . 2_545
H13 H4 2.3791 no . 2_545
H13 H10 3.5452 no . 3_556
H13 H25 2.7551 no . 2_545
H13 H26 2.8318 no . 2_545
H14 F1 3.1710 no . 2_545
H14 O5 3.4676 no . .
H14 C4 3.2949 no . 2_545
H14 H4 2.4587 no . 2_545
H14 H11 3.4436 no . 3_556
H14 H23 2.9268 no . 4_555
H14 H24 3.3946 no . 4_555
H16 O5 2.8964 no . .
H17 O5 2.8228 no . .
H17 C3 3.4908 no . 2_545
H17 C4 3.1288 no . 2_545
H17 C5 3.4476 no . 2_545
H17 H4 3.2110 no . 2_545
H17 H26 3.1302 no . .
H18 O6 2.8527 no . 1_655
H18 C5 3.2463 no . 2_545
H18 C6 3.1080 no . 2_545
H18 C7 3.5001 no . 2_545
H18 H6 3.2752 no . 2_545
H18 H7 3.1071 no . 1_655
H18 H22 3.1622 no . 1_655
H19 O2 2.2804 no . 1_655
H19 O4 2.3981 no . 1_655
H19 O6 2.9328 no . 1_655
H19 C1 3.1944 no . 1_655
H19 C7 3.4777 no . 1_655
H19 C8 3.3576 no . 1_655
H19 H7 2.8302 no . 1_655
H19 H10 3.3649 no . 1_655
H22 F2 3.3372 no . 2_455
H22 O2 3.5609 no . 2_445
H22 C7 3.0146 no . 2_445
H22 H7 2.5791 no . 2_445
H22 H11 2.8835 no . 2_455
H22 H18 3.1622 no . 1_455
H23 F2 3.4411 no . 2_455
H23 O2 3.0580 no . 2_445
H23 O3 2.8230 no . 4_454
H23 N1 3.3442 no . 4_454
H23 C8 3.5890 no . 4_454
H23 C11 3.4040 no . 2_455
H23 C14 3.5306 no . 4_454
H23 H11 2.5932 no . 2_455
H23 H14 2.9268 no . 4_454
H24 F1 2.6321 no . 3_565
H24 N1 3.3194 no . 2_545
H24 N1 3.3004 no . 4_454
H24 C15 2.9031 no . 4_454
H24 C16 3.4122 no . 4_454
H24 C19 3.3752 no . 4_454
H24 C20 2.8896 no . 4_454
H24 H10 3.5467 no . 4_554
H24 H14 3.3946 no . 4_454
H25 F2 3.2411 no . 2_555
H25 O1 3.1427 no . 2_545
H25 O4 2.8929 no . 4_554
H25 N1 3.3596 no . 2_545
H25 C10 3.5744 no . 4_554
H25 C13 3.4316 no . 2_555
H25 H10 2.8793 no . 4_554
H25 H13 2.7550 no . 2_555
H26 F2 3.1427 no . 2_555
H26 C3 3.0693 no . 2_545
H26 C13 3.5796 no . 2_555
H26 H3 2.5176 no . 2_545
H26 H13 2.8318 no . 2_555
H26 H17 3.1302 no . .
data_Ru-pF-Phz-dry
_database_code_depnum_ccdc_archive 'CCDC 895510'
#TrackingRef 'CCDC-895510_R2.cif'
# 5. CHEMICAL DATA
_chemical_name_systematic
; ?
;
_chemical_name_common (Ru2(p-F-PhCO2)4(phz))
# Get _chemical_formula_moiety using checkCIF
_chemical_formula_moiety ?
_chemical_formula_structural ?
_chemical_formula_analytical ?
_chemical_formula_sum 'C40 H24 F4 N2 O8 Ru2'
_chemical_formula_weight 938.760
_chemical_melting_point ?
_chemical_compound_source ? # for minerals and
# natural products
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ru Ru -1.0980 1.0370 'International Tables for Crystallography, Vol. C'
C C 0.0033 0.0021 'International Tables for Crystallography, Vol. C'
O O 0.0113 0.0079 'International Tables for Crystallography, Vol. C'
H H 0.0000 0.0000 'International Tables for Crystallography, Vol. C'
N N 0.0063 0.0043 'International Tables for Crystallography, Vol. C'
F F 0.0186 0.0133 'International Tables for Crystallography, Vol. C'
#===============================================================================
# 6. POWDER SPECIMEN AND CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
_cell_length_a 9.9825(8)
_cell_length_b 10.9906(8)
_cell_length_c 11.4527(7)
_cell_angle_alpha 65.866(5)
_cell_angle_beta 66.143(6)
_cell_angle_gamma 65.088(7)
_cell_volume 998.2(1)
# If checkCIF gives a different Z value, change both
# _chemical_formula_sum and _chemical_formula_weight.
_cell_formula_units_Z 1
_cell_measurement_temperature 195(1)
_cell_special_details ?
_exptl_crystal_density_diffrn 1.5616
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 932.00
# 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 ? # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick ? # parallel to
# scattering vector
# in reflection
# The next five fields are character fields that describe the specimen.
_pd_spec_mounting
# This field should be
# used to give details of the
# container.
; ?
;
_pd_spec_mount_mode reflection
_pd_spec_shape flat_sheet
_pd_char_particle_morphology ?
_pd_char_colour ?
# 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 ?
_exptl_absorpt_coefficient_mu ?
# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_correction_type ? # include if applicable
_exptl_absorpt_process_details ? # include if applicable
_exptl_absorpt_correction_T_min ? # include if applicable
_exptl_absorpt_correction_T_max ? # include if applicable
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
; ?
;
# 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
; ?
;
_pd_calibration_special_details
# description of the method used
# to calibrate the instrument
; ?
;
_diffrn_ambient_temperature 195(1)
_diffrn_source synchrotron
_diffrn_source_target ?
_diffrn_source_type ?
_diffrn_radiation_type synchrotron
_diffrn_measurement_device_type debye-scherrer
_diffrn_detector 'imaging plate'
_diffrn_detector_type ?
_pd_meas_scan_method step
_pd_meas_special_details
; ?
;
_diffrn_radiation_wavelength 0.799020
_diffrn_radiation_monochromator 'Si crystal'
_pd_meas_number_of_points 4701
_pd_meas_2theta_range_min 3.0000
_pd_meas_2theta_range_max 50.0000
_pd_meas_2theta_range_inc 0.0100
#===============================================================================
# 8. 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_calc_method 'Rietveld Refinement'
_pd_proc_ls_profile_function 'split Pearson VII function'
_pd_proc_ls_background_function 'composite background function'
_pd_proc_ls_pref_orient_corr
; none
;
# Replace '; ?' with the following four lines for the March-Dollase function:
#; $P_k = \sum_{j=1}^{m_k} \frac{1}{m_k}
#\left( r^2 \cos^2 \alpha_j +r^{-1}\ sin^2 \alpha_j \right)^{-3/2}$
#with a preferred-orientation vector, (hkl),
#and r = 1.0(0)
_pd_proc_ls_prof_R_factor 0.01836
_pd_proc_ls_prof_wR_factor 0.02733
_pd_proc_ls_prof_wR_expected 0.00661
_refine_ls_R_I_factor 0.01905
_refine_ls_R_Fsqd_factor 0.00901
_refine_ls_R_factor_all 0.00901
_refine_special_details
; ?
;
_refine_ls_matrix_type full
_refine_ls_weighting_scheme sigma
_refine_ls_weighting_details 1/y~i~
_refine_ls_hydrogen_treatment riding
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_parameters 91
_refine_ls_number_restraints 0
_refine_ls_number_constraints 26
# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all 4.1355
_refine_ls_restrained_S_all ?
# The following item can be obtained by setting NPRINT at 2 in *.ins.
_refine_ls_shift/su_max 0.0
_refine_ls_shift/su_mean ?
_refine_diff_density_max 0.0
_refine_diff_density_min 0.0
# 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 3.0000
_pd_proc_2theta_range_max 50.0000
_pd_proc_2theta_range_inc 0.0100
_pd_proc_wavelength ?
# Each refinement must be accompanied by a listing of the powder data
# in CIF format. Each listing should be sent as a separate file consisting
# of one data block containing a single powder profile. The value of
# _pd_block_diffractogram_id is used to associate each refinement with
# its corresponding powder profile, since it must match the value
# of _pd_block_id in the file containing the powder data. A template
# for supplying powder data in CIF format is available by ftp at
# ftp://ftp.iucr.org/pub/rietdataform.cif and an example is given
# at ftp://ftp.iucr.org/pub/rietdataxmpl.cif.
_pd_block_diffractogram_id ?
# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions ?
_pd_proc_info_data_reduction ?
# The following items are used to identify the programs used.
_computing_data_collection ?
_computing_cell_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_data_reduction ?
_computing_structure_solution FOX
_computing_structure_refinement 'RIETAN-FP (Izumi and Momma, 2007)'
_computing_molecular_graphics 'VESTA (Momma and Izumi, 2008)'
_computing_publication_material ?
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_adp_type
_atom_site_U_iso_or_equiv
_atom_site_type_symbol
C1 0.346(7) 0.731(6) 0.075(7) 1 2 i Uiso 0.0094 C
C2 0.252(7) 0.863(6) 0.114(7) 1 2 i Uiso 0.0094 C
C3 0.096(8) 0.898(7) 0.157(7) 1 2 i Uiso 0.0094 C
C4 0.005(7) 0.018(7) 0.194(6) 1 2 i Uiso 0.0094 C
C5 0.077(7) 0.101(6) 0.189(7) 1 2 i Uiso 0.0094 C
C6 0.231(8) 0.073(7) 0.146(7) 1 2 i Uiso 0.0094 C
C7 0.325(7) 0.953(7) 0.106(6) 1 2 i Uiso 0.0094 C
C8 0.491(9) 0.331(8) 0.241(5) 1 2 i Uiso 0.0094 C
C9 0.477(8) 0.246(6) 0.381(6) 1 2 i Uiso 0.0094 C
C10 0.595(8) 0.211(8) 0.438(7) 1 2 i Uiso 0.0094 C
C11 0.580(8) 0.134(7) 0.567(7) 1 2 i Uiso 0.0094 C
C12 0.446(8) 0.091(5) 0.636(5) 1 2 i Uiso 0.0094 C
C13 0.332(7) 0.129(7) 0.579(7) 1 2 i Uiso 0.0094 C
C14 0.349(8) 0.206(7) 0.450(6) 1 2 i Uiso 0.0094 C
C15 0.024(9) 0.505(7) 0.111(7) 1 2 i Uiso 0.0094 C
C16 0.042(7) 0.516(7) 0.224(7) 1 2 i Uiso 0.0094 C
C17 0.081(8) 0.433(6) 0.684(6) 1 2 i Uiso 0.0094 C
C18 0.229(7) 0.394(7) 0.696(6) 1 2 i Uiso 0.0094 C
C19 0.255(7) 0.403(6) 0.801(6) 1 2 i Uiso 0.0094 C
C20 0.127(8) 0.454(7) 0.904(7) 1 2 i Uiso 0.0094 C
O1 0.274(5) 0.664(4) 0.070(4) 1 2 i Uiso 0.0094 O
O2 0.488(5) 0.694(5) 0.046(4) 1 2 i Uiso 0.0094 O
O3 0.371(5) 0.389(4) 0.205(4) 1 2 i Uiso 0.0094 O
O4 0.607(4) 0.370(5) 0.179(4) 1 2 i Uiso 0.0094 O
F1 -0.011(4) 0.218(3) 0.227(3) 1 2 i Uiso 0.0094 F
F2 0.429(4) 0.010(3) 0.768(3) 1 2 i Uiso 0.0094 F
N1 0.151(6) 0.457(5) 0.013(6) 1 2 i Uiso 0.0094 N
Ru1 0.388(1) 0.489(1) 0.006(1) 1 2 i Uiso 0.01361 Ru
H3 0.04924 0.83724 0.16065 1 2 i Uiso 0.01129 H
H4 -0.10392 0.04013 0.22458 1 2 i Uiso 0.01129 H
H6 0.27839 0.13424 0.14169 1 2 i Uiso 0.01129 H
H7 0.43367 0.93085 0.07603 1 2 i Uiso 0.01129 H
H10 0.68477 0.23929 0.3901 1 2 i Uiso 0.01129 H
H11 0.65854 0.10944 0.60673 1 2 i Uiso 0.01129 H
H13 0.24239 0.1002 0.62682 1 2 i Uiso 0.01129 H
H14 0.2706 0.23007 0.41015 1 2 i Uiso 0.01129 H
H16 0.14249 0.48945 0.23249 1 2 i Uiso 0.01129 H
H17 0.06606 0.42585 0.61041 1 2 i Uiso 0.01129 H
H18 0.31596 0.35923 0.62938 1 2 i Uiso 0.01129 H
H19 0.35555 0.37642 0.80913 1 2 i Uiso 0.01129 H
#===============================================================================
#10. GEOMETRICAL PARAMETERS
_geom_special_details ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C2 C3 1.35(8) . 1_555 ?
C2 C7 1.41(7) . 1_555 ?
C3 C4 1.37(8) . 1_565 ?
C1 O1 1.24(6) . 1_555 ?
C1 O2 1.24(6) . 1_555 ?
C1 C2 1.50(6) . 1_555 ?
C4 C5 1.35(7) . 1_555 ?
C6 C7 1.39(8) . 1_545 ?
C5 F1 1.34(5) . 1_555 ?
C5 C6 1.35(8) . 1_555 ?
O2 Ru1 2.05(4) . 2_665 ?
O1 Ru1 2.05(4) . 1_555 ?
C9 C14 1.35(7) . 1_555 ?
C9 C10 1.41(8) . 1_555 ?
C10 C11 1.35(9) . 1_555 ?
C8 O4 1.24(6) . 1_555 ?
C8 O3 1.24(7) . 1_555 ?
C8 C9 1.48(7) . 1_555 ?
C13 C14 1.35(7) . 1_555 ?
C11 C12 1.41(7) . 1_555 ?
C12 C13 1.38(7) . 1_555 ?
C12 F2 1.38(5) . 1_555 ?
C12 C11 1.41(7) . 1_555 ?
O4 Ru1 2.05(4) . 2_665 ?
O3 Ru1 2.05(4) . 1_555 ?
N1 Ru1 2.50(5) . 1_555 ?
C15 N1 1.38(8) . 1_555 ?
C15 C16 1.44(7) . 1_555 ?
C15 C20 1.44(5) . 2_566 ?
C20 N1 1.38(8) . 1_556 ?
C19 C20 1.43(7) . 1_555 ?
C18 C19 1.38(7) . 1_555 ?
C17 C18 1.40(7) . 1_555 ?
C16 C17 1.34(8) . 2_566 ?
Ru1 Ru1 2.29(1) . 2_665 ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C3 C2 C7 119(5) 1_555 . 1_555 ?
C3 C2 C1 120(7) 1_555 . 1_555 ?
C7 C2 C1 120(6) 1_555 . 1_555 ?
O1 C2 C4 121(4) 1_555 . 1_565 ?
O2 C2 C6 124(4) 1_555 . 1_565 ?
C2 C3 C4 123(7) 1_555 . 1_565 ?
C5 C3 C1 123(4) 1_565 . 1_555 ?
C6 C3 O1 120(4) 1_565 . 1_555 ?
C6 C7 C2 117(6) 1_565 . 1_555 ?
C5 C7 C1 119(3) 1_565 . 1_555 ?
C4 C7 O2 116(3) 1_565 . 1_555 ?
O1 C1 O2 123(5) 1_555 . 1_555 ?
O1 C1 C2 117(6) 1_555 . 1_555 ?
O2 C1 C2 120(7) 1_555 . 1_555 ?
C5 C4 C3 117(6) 1_555 . 1_545 ?
C5 C6 C7 120(7) 1_555 . 1_545 ?
F1 C6 C2 119(3) 1_555 . 1_545 ?
F1 C5 C4 118(6) 1_555 . 1_555 ?
F1 C5 C6 119(7) 1_555 . 1_555 ?
C4 C5 C6 123(6) 1_555 . 1_555 ?
C1 O2 Ru1 119(4) 1_555 . 2_665 ?
C1 O1 Ru1 121(4) 1_555 . 1_555 ?
C14 C9 C10 123(6) 1_555 . 1_555 ?
C14 C9 C8 117(6) 1_555 . 1_555 ?
C10 C9 C8 120(7) 1_555 . 1_555 ?
C13 C9 O3 120(4) 1_555 . 1_555 ?
O4 C9 C11 121(4) 1_555 . 1_555 ?
C13 C14 C9 119(6) 1_555 . 1_555 ?
C12 C14 C8 121(4) 1_555 . 1_555 ?
O3 C14 C11 117(4) 1_555 . 1_555 ?
C11 C10 C9 119(7) 1_555 . 1_555 ?
C12 C10 C8 118(4) 1_555 . 1_555 ?
O4 C10 C13 115(3) 1_555 . 1_555 ?
O4 C8 O3 123(5) 1_555 . 1_555 ?
O4 C8 C9 117(6) 1_555 . 1_555 ?
O3 C8 C9 117(7) 1_555 . 1_555 ?
C14 C13 C12 119(6) 1_555 . 1_555 ?
C9 C13 F2 119(4) 1_555 . 1_555 ?
C10 C11 C12 117(6) 1_555 . 1_555 ?
C9 C11 F2 116(4) 1_555 . 1_555 ?
C13 C12 F2 119(6) 1_555 . 1_555 ?
C13 C12 C11 123(5) 1_555 . 1_555 ?
F2 C12 C11 118(6) 1_555 . 1_555 ?
C8 O4 Ru1 117(4) 1_555 . 2_665 ?
C8 O3 Ru1 119(4) 1_555 . 1_555 ?
C16 O3 Ru1 124(2) 1_555 . 2_665 ?
C15 N1 C20 118(4) 1_555 . 1_554 ?
C20 N1 Ru1 124(5) 1_554 . 1_555 ?
C20 N1 C19 118(4) 2_566 . 1_554 ?
C16 N1 C15 119(4) 1_555 . 2_565 ?
N1 C15 C16 121(7) 1_555 . 1_555 ?
N1 C15 C20 119(7) 1_555 . 2_566 ?
C16 C15 C20 120(8) 1_555 . 2_566 ?
C20 C15 C19 119(5) 1_554 . 2_566 ?
C17 C15 N1 119(4) 2_566 . 2_565 ?
C18 C15 C15 118(5) 2_566 . 2_565 ?
N1 C20 C19 120(7) 1_556 . 1_555 ?
N1 C20 C15 123(7) 1_556 . 2_566 ?
C19 C20 C15 117(8) 1_555 . 2_566 ?
C15 C20 C16 122(5) 1_556 . 2_566 ?
N1 C20 C18 117(4) 2_566 . 1_555 ?
C18 C19 C20 119(7) 1_555 . 1_555 ?
N1 C19 C17 120(4) 1_556 . 1_555 ?
C19 C18 C17 123(6) 1_555 . 1_555 ?
C16 C17 C18 120(7) 2_566 . 1_555 ?
C17 C16 C15 120(7) 2_566 . 1_555 ?
C17 C16 O1 120(4) 2_566 . 1_555 ?
C18 C16 N1 118(3) 2_566 . 1_555 ?
data_Ru-pF-phz_1
_database_code_depnum_ccdc_archive 'CCDC 895511'
#TrackingRef 'Ru-pF-phz.cif'
#==============================================================================
# CHEMICAL DATA
_chemical_formula_sum 'C52 H34 F4 N4 O12 Ru2'
_chemical_formula_moiety 'C52 H34 F4 N4 O12 Ru2'
_chemical_formula_weight 1184.99
_chemical_melting_point ?
#==============================================================================
# CRYSTAL DATA
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M 'P 1 21/n 1'
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 1/2+X,1/2-Y,1/2+Z
#------------------------------------------------------------------------------
_cell_length_a 10.064(3)
_cell_length_b 11.778(4)
_cell_length_c 20.097(6)
_cell_angle_alpha 90.0000
_cell_angle_beta 91.221(5)
_cell_angle_gamma 90.0000
_cell_volume 2381.6(13)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6416
_cell_measurement_theta_min 3.30
_cell_measurement_theta_max 27.50
_cell_measurement_temperature 93
#------------------------------------------------------------------------------
_exptl_crystal_description block
_exptl_crystal_colour brown
_exptl_crystal_size_max 0.130
_exptl_crystal_size_mid 0.110
_exptl_crystal_size_min 0.100
_exptl_crystal_density_diffrn 1.652
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1188.00
_exptl_absorpt_coefficient_mu 0.720
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details 'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min 0.733
_exptl_absorpt_correction_T_max 0.931
#==============================================================================
# EXPERIMENTAL DATA
_diffrn_ambient_temperature 93
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71075
_diffrn_measurement_device_type 'Rigaku Saturn724'
_diffrn_measurement_method \w
_diffrn_detector_area_resol_mean 7.111
_diffrn_reflns_number 18812
_diffrn_reflns_av_R_equivalents 0.0549
_diffrn_reflns_theta_max 27.48
_diffrn_reflns_theta_full 27.48
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 11
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_limit_l_max 26
_diffrn_standards_number 0
_diffrn_standards_interval_count .
_diffrn_standards_decay_% ?
#==============================================================================
# REFINEMENT DATA
_refine_special_details
;
Refinement was performed using all reflections. The weighted
R-factor (wR) and goodness of fit (S) are based on F^2^.
R-factor (gt) are based on F. The threshold expression of
F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt).
;
_reflns_number_total 5424
_reflns_number_gt 3436
_reflns_threshold_expression F^2^>2.0\s(F^2^)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_gt 0.0941
_refine_ls_wR_factor_ref 0.2245
_refine_ls_number_restraints 306
_refine_ls_hydrogen_treatment constr
_refine_ls_number_reflns 5424
_refine_ls_number_parameters 334
_refine_ls_goodness_of_fit_ref 1.249
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0134P)^2^+46.5717P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_refine_ls_shift/su_max 0.000
_refine_diff_density_max 2.350
_refine_diff_density_min -1.310
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
F F 0.0171 0.0103
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ru Ru -1.2594 0.8363
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS
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
Ru1 Ru 0.11351(7) 0.50416(7) 0.49927(3) 0.01750(19) Uani 1.0 4 d . . .
F1 F -0.0351(10) 0.6152(8) 0.0986(4) 0.070(3) Uani 1.0 4 d . . .
F2 F 0.0311(9) -0.1659(6) 0.3770(5) 0.064(3) Uani 1.0 4 d . . .
O1 O 0.1005(6) 0.5603(5) 0.4018(3) 0.0174(12) Uani 1.0 4 d . . .
O2 O -0.1205(6) 0.5527(6) 0.4039(3) 0.0166(12) Uani 1.0 4 d . . .
O3 O 0.1180(6) 0.3361(6) 0.4685(3) 0.0169(12) Uani 1.0 4 d . . .
O4 O -0.1049(6) 0.3292(6) 0.4700(3) 0.0193(13) Uani 1.0 4 d . . .
O5 O 0.1092(10) 0.3020(8) 0.2896(5) 0.052(3) Uani 1.0 4 d . . .
O6 O -0.1051(10) 0.2964(8) 0.2895(5) 0.050(2) Uani 1.0 4 d . . .
N1 N 0.3569(6) 0.5056(7) 0.4991(4) 0.0133(12) Uani 1.0 4 d . . .
N2 N -0.0010(11) 0.2939(9) 0.2620(5) 0.0389(18) Uani 1.0 4 d . . .
C1 C -0.0139(9) 0.5646(8) 0.3752(5) 0.0188(15) Uani 1.0 4 d . . .
C2 C -0.0191(10) 0.5840(9) 0.3006(5) 0.0247(17) Uani 1.0 4 d . . .
C3 C 0.0959(12) 0.5977(9) 0.2670(6) 0.033(2) Uani 1.0 4 d . . .
C4 C 0.0912(14) 0.6085(10) 0.1970(6) 0.043(3) Uani 1.0 4 d . . .
C5 C -0.0289(15) 0.6048(11) 0.1668(6) 0.048(3) Uani 1.0 4 d . . .
C6 C -0.1452(14) 0.5920(11) 0.1988(6) 0.042(3) Uani 1.0 4 d . . .
C7 C -0.1394(11) 0.5805(9) 0.2678(5) 0.0303(19) Uani 1.0 4 d . . .
C8 C 0.0091(9) 0.2873(8) 0.4613(4) 0.0192(15) Uani 1.0 4 d . . .
C9 C 0.0140(10) 0.1641(9) 0.4388(5) 0.0243(17) Uani 1.0 4 d . . .
C10 C -0.1006(11) 0.1008(9) 0.4343(5) 0.0305(19) Uani 1.0 4 d . . .
C11 C -0.0936(13) -0.0141(10) 0.4129(6) 0.040(2) Uani 1.0 4 d . . .
C12 C 0.0265(15) -0.0547(10) 0.3976(7) 0.047(3) Uani 1.0 4 d . . .
C13 C 0.1426(13) 0.0046(11) 0.4025(7) 0.046(3) Uani 1.0 4 d . . .
C14 C 0.1341(12) 0.1163(9) 0.4224(6) 0.035(2) Uani 1.0 4 d . . .
C15 C 0.4293(8) 0.4661(7) 0.4456(5) 0.0154(15) Uani 1.0 4 d . . .
C16 C 0.3588(9) 0.4311(8) 0.3871(5) 0.0203(17) Uani 1.0 4 d . . .
C17 C 0.4263(9) 0.3918(9) 0.3339(5) 0.0214(17) Uani 1.0 4 d . . .
C18 C 0.5624(9) 0.3831(9) 0.3359(5) 0.0223(17) Uani 1.0 4 d . . .
C19 C 0.6333(9) 0.4142(8) 0.3917(5) 0.0204(17) Uani 1.0 4 d . . .
C20 C 0.5676(8) 0.4582(8) 0.4478(5) 0.0156(15) Uani 1.0 4 d . . .
C21 C -0.0004(10) 0.2802(9) 0.1874(6) 0.0284(17) Uani 1.0 4 d . . .
C22 C -0.1225(10) 0.2717(8) 0.1552(6) 0.0277(18) Uani 1.0 4 d . . .
C23 C -0.1226(12) 0.2613(9) 0.0863(6) 0.035(2) Uani 1.0 4 d . . .
C24 C -0.0056(12) 0.2604(9) 0.0531(6) 0.037(2) Uani 1.0 4 d . . .
C25 C 0.1136(12) 0.2650(9) 0.0866(6) 0.036(2) Uani 1.0 4 d . . .
C26 C 0.1151(10) 0.2765(9) 0.1560(6) 0.0298(19) Uani 1.0 4 d . . .
H3 H 0.1787 0.5999 0.2906 0.0396 Uiso 1.0 4 calc R . .
H4 H 0.1699 0.6180 0.1724 0.0511 Uiso 1.0 4 calc R . .
H6 H -0.2278 0.5910 0.1750 0.0505 Uiso 1.0 4 calc R . .
H7 H -0.2187 0.5704 0.2919 0.0364 Uiso 1.0 4 calc R . .
H10 H -0.1837 0.1335 0.4452 0.0366 Uiso 1.0 4 calc R . .
H11 H -0.1709 -0.0603 0.4096 0.0481 Uiso 1.0 4 calc R . .
H13 H 0.2255 -0.0295 0.3926 0.0554 Uiso 1.0 4 calc R . .
H14 H 0.2125 0.1612 0.4248 0.0415 Uiso 1.0 4 calc R . .
H16 H 0.2645 0.4351 0.3851 0.0244 Uiso 1.0 4 calc R . .
H17 H 0.3784 0.3700 0.2946 0.0257 Uiso 1.0 4 calc R . .
H18 H 0.6076 0.3553 0.2982 0.0267 Uiso 1.0 4 calc R . .
H19 H 0.7273 0.4062 0.3929 0.0245 Uiso 1.0 4 calc R . .
H22 H -0.2029 0.2729 0.1791 0.0333 Uiso 1.0 4 calc R . .
H23 H -0.2045 0.2547 0.0623 0.0416 Uiso 1.0 4 calc R . .
H24 H -0.0073 0.2565 0.0059 0.0441 Uiso 1.0 4 calc R . .
H25 H 0.1944 0.2604 0.0631 0.0435 Uiso 1.0 4 calc R . .
H26 H 0.1969 0.2816 0.1803 0.0357 Uiso 1.0 4 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Ru1 0.0157(4) 0.0226(4) 0.0142(3) 0.0005(4) 0.0000(3) -0.0038(3)
F1 0.119(7) 0.070(5) 0.021(3) 0.015(5) 0.006(4) 0.007(4)
F2 0.098(6) 0.020(4) 0.075(5) -0.002(4) 0.018(5) -0.009(4)
O1 0.007(3) 0.023(3) 0.022(3) -0.003(3) 0.008(3) 0.000(3)
O2 0.006(3) 0.025(3) 0.019(3) 0.001(3) -0.003(3) -0.001(3)
O3 0.006(3) 0.024(3) 0.020(3) 0.001(3) 0.001(3) -0.003(3)
O4 0.009(3) 0.028(4) 0.021(3) -0.004(3) -0.001(3) -0.002(3)
O5 0.057(5) 0.055(5) 0.043(5) -0.016(5) -0.017(4) 0.008(4)
O6 0.058(5) 0.054(5) 0.039(5) -0.007(5) 0.010(4) 0.007(4)
N1 0.012(3) 0.014(3) 0.014(3) 0.002(3) 0.001(3) -0.006(3)
N2 0.044(5) 0.036(4) 0.036(4) -0.006(4) -0.003(4) 0.009(4)
C1 0.012(4) 0.018(4) 0.026(4) -0.003(3) -0.002(3) -0.003(3)
C2 0.026(4) 0.023(4) 0.025(4) 0.002(4) 0.002(3) -0.001(4)
C3 0.035(5) 0.031(5) 0.033(4) 0.001(4) 0.009(4) 0.002(4)
C4 0.056(5) 0.038(5) 0.035(5) 0.006(5) 0.015(4) 0.007(5)
C5 0.075(6) 0.045(5) 0.024(4) 0.010(5) 0.004(4) 0.006(4)
C6 0.057(5) 0.043(5) 0.026(4) 0.009(5) -0.009(4) 0.002(4)
C7 0.036(5) 0.032(5) 0.024(4) 0.005(4) -0.001(4) 0.001(4)
C8 0.013(4) 0.028(4) 0.016(4) -0.001(3) 0.004(3) 0.001(3)
C9 0.026(4) 0.027(4) 0.020(4) -0.002(3) 0.002(4) 0.002(4)
C10 0.029(5) 0.031(4) 0.031(5) -0.003(4) -0.002(4) -0.002(4)
C11 0.054(5) 0.025(5) 0.042(5) -0.010(4) 0.001(5) 0.000(4)
C12 0.071(5) 0.019(4) 0.052(5) -0.002(4) 0.013(5) -0.000(4)
C13 0.055(5) 0.027(5) 0.056(6) 0.006(4) 0.012(5) -0.003(5)
C14 0.034(5) 0.026(4) 0.044(5) 0.001(4) 0.009(4) -0.002(4)
C15 0.005(3) 0.020(4) 0.022(4) -0.004(3) -0.000(3) -0.004(3)
C16 0.004(4) 0.033(5) 0.023(4) -0.003(4) 0.001(3) -0.009(4)
C17 0.011(4) 0.032(5) 0.022(4) -0.002(4) 0.001(3) -0.009(4)
C18 0.010(4) 0.032(5) 0.025(4) -0.000(4) 0.002(3) -0.008(4)
C19 0.008(4) 0.027(4) 0.026(4) -0.006(3) 0.003(3) -0.008(4)
C20 0.005(3) 0.019(4) 0.022(4) -0.003(3) -0.003(3) -0.004(3)
C21 0.026(4) 0.023(4) 0.036(4) -0.001(4) -0.001(3) 0.006(4)
C22 0.021(4) 0.021(4) 0.041(5) 0.001(4) -0.001(4) -0.000(4)
C23 0.036(5) 0.026(5) 0.042(5) 0.003(4) -0.009(4) -0.005(4)
C24 0.045(5) 0.024(5) 0.042(5) -0.002(4) 0.002(4) -0.008(4)
C25 0.035(5) 0.025(5) 0.049(5) -0.001(4) 0.009(4) -0.005(5)
C26 0.019(4) 0.024(5) 0.046(5) -0.001(4) 0.000(4) 0.004(4)
#==============================================================================
_computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'
_computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4'
_computing_data_reduction 'CrystalClear-SM Expert 2.0 r4'
_computing_structure_solution 'Il Milione (Burla, et al., 2007)'
_computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_molecular_graphics 'CrystalStructure 4.0'
#==============================================================================
# MOLECULAR GEOMETRY
_geom_special_details
;
ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Ru1 Ru1 2.2876(12) yes . 3_566
Ru1 O1 2.069(6) yes . .
Ru1 O2 2.057(6) yes . 3_566
Ru1 O3 2.075(7) yes . .
Ru1 O4 2.060(7) yes . 3_566
Ru1 N1 2.450(7) yes . .
F1 C5 1.376(14) yes . .
F2 C12 1.375(14) yes . .
O1 C1 1.260(11) yes . .
O2 C1 1.238(11) yes . .
O3 C8 1.243(11) yes . .
O4 C8 1.264(11) yes . .
O5 N2 1.232(14) yes . .
O6 N2 1.196(14) yes . .
N1 C15 1.392(11) yes . .
N1 C20 1.365(11) yes . 3_666
N2 C21 1.508(15) yes . .
C1 C2 1.516(14) yes . .
C2 C3 1.362(15) yes . .
C2 C7 1.366(15) yes . .
C3 C4 1.412(16) yes . .
C4 C5 1.34(2) yes . .
C5 C6 1.36(2) yes . .
C6 C7 1.393(15) yes . .
C8 C9 1.520(14) yes . .
C9 C10 1.375(15) yes . .
C9 C14 1.381(15) yes . .
C10 C11 1.422(16) yes . .
C11 C12 1.342(19) yes . .
C12 C13 1.363(19) yes . .
C13 C14 1.378(17) yes . .
C15 C16 1.422(12) yes . .
C15 C20 1.395(11) yes . .
C16 C17 1.360(13) yes . .
C17 C18 1.374(13) yes . .
C18 C19 1.366(13) yes . .
C19 C20 1.417(13) yes . .
C21 C22 1.380(15) yes . .
C21 C26 1.335(15) yes . .
C22 C23 1.389(16) yes . .
C23 C24 1.367(17) yes . .
C24 C25 1.363(17) yes . .
C25 C26 1.403(17) yes . .
C3 H3 0.950 no . .
C4 H4 0.950 no . .
C6 H6 0.950 no . .
C7 H7 0.950 no . .
C10 H10 0.950 no . .
C11 H11 0.950 no . .
C13 H13 0.950 no . .
C14 H14 0.950 no . .
C16 H16 0.950 no . .
C17 H17 0.950 no . .
C18 H18 0.950 no . .
C19 H19 0.950 no . .
C22 H22 0.950 no . .
C23 H23 0.950 no . .
C24 H24 0.950 no . .
C25 H25 0.950 no . .
C26 H26 0.950 no . .
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
Ru1 Ru1 O1 89.01(16) yes 3_566 . .
Ru1 Ru1 O2 89.32(16) yes 3_566 . 3_566
Ru1 Ru1 O3 89.48(16) yes 3_566 . .
Ru1 Ru1 O4 89.34(16) yes 3_566 . 3_566
Ru1 Ru1 N1 177.84(18) yes 3_566 . .
O1 Ru1 O2 178.3(3) yes . . 3_566
O1 Ru1 O3 91.4(3) yes . . .
O1 Ru1 O4 88.7(3) yes . . 3_566
O1 Ru1 N1 92.3(3) yes . . .
O2 Ru1 O3 88.3(3) yes 3_566 . .
O2 Ru1 O4 91.6(3) yes 3_566 . 3_566
O2 Ru1 N1 89.4(3) yes 3_566 . .
O3 Ru1 O4 178.8(3) yes . . 3_566
O3 Ru1 N1 88.8(3) yes . . .
O4 Ru1 N1 92.4(3) yes 3_566 . .
Ru1 O1 C1 117.0(6) yes . . .
Ru1 O2 C1 117.8(6) yes 3_566 . .
Ru1 O3 C8 116.8(6) yes . . .
Ru1 O4 C8 117.2(6) yes 3_566 . .
Ru1 N1 C15 122.6(5) yes . . .
Ru1 N1 C20 122.8(5) yes . . 3_666
C15 N1 C20 114.6(7) yes . . 3_666
O5 N2 O6 125.4(10) yes . . .
O5 N2 C21 115.7(10) yes . . .
O6 N2 C21 119.0(10) yes . . .
O1 C1 O2 126.2(9) yes . . .
O1 C1 C2 116.0(8) yes . . .
O2 C1 C2 117.8(8) yes . . .
C1 C2 C3 119.7(9) yes . . .
C1 C2 C7 119.0(9) yes . . .
C3 C2 C7 121.2(10) yes . . .
C2 C3 C4 119.6(11) yes . . .
C3 C4 C5 117.3(12) yes . . .
F1 C5 C4 118.0(12) yes . . .
F1 C5 C6 117.4(12) yes . . .
C4 C5 C6 124.6(11) yes . . .
C5 C6 C7 117.7(12) yes . . .
C2 C7 C6 119.7(11) yes . . .
O3 C8 O4 127.1(9) yes . . .
O3 C8 C9 116.2(8) yes . . .
O4 C8 C9 116.6(8) yes . . .
C8 C9 C10 120.3(9) yes . . .
C8 C9 C14 119.6(9) yes . . .
C10 C9 C14 120.0(10) yes . . .
C9 C10 C11 119.3(10) yes . . .
C10 C11 C12 117.4(11) yes . . .
F2 C12 C11 116.4(12) yes . . .
F2 C12 C13 118.3(12) yes . . .
C11 C12 C13 125.2(12) yes . . .
C12 C13 C14 116.8(12) yes . . .
C9 C14 C13 121.3(11) yes . . .
N1 C15 C16 118.4(7) yes . . .
N1 C15 C20 122.5(8) yes . . .
C16 C15 C20 119.1(8) yes . . .
C15 C16 C17 120.0(8) yes . . .
C16 C17 C18 121.1(9) yes . . .
C17 C18 C19 120.5(9) yes . . .
C18 C19 C20 120.4(8) yes . . .
N1 C20 C15 122.8(8) yes 3_666 . .
N1 C20 C19 118.3(7) yes 3_666 . .
C15 C20 C19 118.8(8) yes . . .
N2 C21 C22 116.9(9) yes . . .
N2 C21 C26 119.7(10) yes . . .
C22 C21 C26 123.5(10) yes . . .
C21 C22 C23 117.1(10) yes . . .
C22 C23 C24 120.3(11) yes . . .
C23 C24 C25 121.1(11) yes . . .
C24 C25 C26 119.1(11) yes . . .
C21 C26 C25 118.8(10) yes . . .
C2 C3 H3 120.202 no . . .
C4 C3 H3 120.224 no . . .
C3 C4 H4 121.350 no . . .
C5 C4 H4 121.352 no . . .
C5 C6 H6 121.178 no . . .
C7 C6 H6 121.164 no . . .
C2 C7 H7 120.144 no . . .
C6 C7 H7 120.164 no . . .
C9 C10 H10 120.348 no . . .
C11 C10 H10 120.349 no . . .
C10 C11 H11 121.325 no . . .
C12 C11 H11 121.324 no . . .
C12 C13 H13 121.590 no . . .
C14 C13 H13 121.591 no . . .
C9 C14 H14 119.365 no . . .
C13 C14 H14 119.365 no . . .
C15 C16 H16 119.988 no . . .
C17 C16 H16 119.989 no . . .
C16 C17 H17 119.442 no . . .
C18 C17 H17 119.456 no . . .
C17 C18 H18 119.739 no . . .
C19 C18 H18 119.736 no . . .
C18 C19 H19 119.818 no . . .
C20 C19 H19 119.803 no . . .
C21 C22 H22 121.441 no . . .
C23 C22 H22 121.447 no . . .
C22 C23 H23 119.827 no . . .
C24 C23 H23 119.837 no . . .
C23 C24 H24 119.440 no . . .
C25 C24 H24 119.448 no . . .
C24 C25 H25 120.464 no . . .
C26 C25 H25 120.466 no . . .
C21 C26 H26 120.583 no . . .
C25 C26 H26 120.593 no . . .
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_publ_flag
_geom_contact_site_symmetry_1
_geom_contact_site_symmetry_2
Ru1 C16 3.486(9) no . .
Ru1 C19 3.461(9) no . 3_666
F2 C14 3.593(13) no . .
O1 C3 2.743(13) no . .
O1 C7 3.586(12) no . .
O1 C8 3.559(11) no . .
O1 C8 3.484(11) no . 3_566
O1 C15 3.582(10) no . .
O1 C16 3.032(11) no . .
O2 C3 3.585(13) no . .
O2 C7 2.758(12) no . .
O2 C8 3.570(11) no . .
O2 C8 3.466(11) no . 3_566
O3 C1 3.524(11) no . .
O3 C1 3.531(11) no . 3_566
O3 C10 3.596(12) no . .
O3 C14 2.756(13) no . .
O3 C15 3.526(10) no . .
O3 C16 3.158(11) no . .
O4 C1 3.498(11) no . .
O4 C1 3.537(11) no . 3_566
O4 C10 2.785(13) no . .
O5 C22 3.549(14) no . .
O5 C26 2.703(14) no . .
O6 C22 2.718(14) no . .
O6 C26 3.524(14) no . .
N1 N1 2.883(9) no . 3_666
C2 C5 2.700(15) no . .
C3 C6 2.763(17) no . .
C4 C7 2.767(17) no . .
C9 C12 2.711(15) no . .
C10 C13 2.785(17) no . .
C11 C14 2.762(17) no . .
C15 C15 2.703(12) no . 3_666
C15 C18 2.782(13) no . .
C16 C19 2.770(12) no . .
C17 C20 2.781(13) no . .
C20 C20 2.711(12) no . 3_666
C21 C24 2.709(16) no . .
C22 C25 2.773(16) no . .
C23 C26 2.752(16) no . .
F1 C18 3.432(13) no . 2_555
F1 C24 3.415(14) no . 3_565
F2 O1 3.334(10) no . 1_545
F2 C1 3.206(11) no . 1_545
F2 C2 3.355(12) no . 1_545
F2 C8 3.582(12) no . 3_556
O1 F2 3.334(10) no . 1_565
O2 C19 2.972(11) no . 1_455
O2 C20 3.462(10) no . 1_455
O2 C23 3.574(13) no . 2_455
O4 C19 3.201(11) no . 1_455
O5 C2 3.572(14) no . .
O5 C3 3.514(15) no . .
O5 C9 3.560(13) no . .
O5 C14 3.455(15) no . .
O5 C16 3.500(13) no . .
O5 C17 3.460(13) no . .
O6 C2 3.502(14) no . .
O6 C6 3.491(16) no . 2_445
O6 C7 3.392(14) no . .
O6 C9 3.566(13) no . .
N1 C24 3.523(13) no . 2_555
N1 C24 3.584(13) no . 4_555
N1 C25 3.522(13) no . 2_555
N2 C2 3.509(14) no . .
C1 F2 3.206(11) no . 1_565
C2 F2 3.355(12) no . 1_565
C2 O5 3.572(14) no . .
C2 O6 3.502(14) no . .
C2 N2 3.509(14) no . .
C3 O5 3.514(15) no . .
C4 C13 3.591(19) no . 2_555
C4 C17 3.398(16) no . 2_555
C5 C17 3.535(17) no . 2_555
C5 C18 3.296(17) no . 2_555
C6 O6 3.491(16) no . 2_455
C7 O6 3.392(14) no . .
C8 F2 3.582(12) no . 3_556
C9 O5 3.560(13) no . .
C9 O6 3.566(13) no . .
C9 C11 3.541(15) no . 3_556
C9 C12 3.562(16) no . 3_556
C10 C12 3.487(17) no . 3_556
C10 C13 3.542(17) no . 3_556
C11 C9 3.541(15) no . 3_556
C11 C14 3.554(16) no . 3_556
C12 C9 3.562(16) no . 3_556
C12 C10 3.487(17) no . 3_556
C13 C4 3.591(19) no . 2_545
C13 C10 3.542(17) no . 3_556
C14 O5 3.455(15) no . .
C14 C11 3.554(16) no . 3_556
C15 C24 3.550(14) no . 2_555
C15 C24 3.486(14) no . 4_555
C16 O5 3.500(13) no . .
C17 O5 3.460(13) no . .
C17 C4 3.398(16) no . 2_545
C17 C5 3.535(17) no . 2_545
C18 F1 3.432(13) no . 2_545
C18 C5 3.296(17) no . 2_545
C19 O2 2.972(11) no . 1_655
C19 O4 3.201(11) no . 1_655
C20 O2 3.462(10) no . 1_655
C20 C24 3.422(14) no . 4_555
C23 O2 3.574(13) no . 2_445
C24 F1 3.415(14) no . 3_565
C24 N1 3.523(13) no . 2_545
C24 N1 3.584(13) no . 4_454
C24 C15 3.550(14) no . 2_545
C24 C15 3.486(14) no . 4_454
C24 C20 3.422(14) no . 4_454
C25 N1 3.522(13) no . 2_545
Ru1 H16 2.8946 no . .
Ru1 H19 2.8686 no . 3_666
F1 H4 2.5149 no . .
F1 H6 2.5157 no . .
F2 H11 2.4834 no . .
F2 H13 2.5454 no . .
O1 H3 2.4309 no . .
O1 H16 2.2435 no . .
O2 H7 2.4477 no . .
O3 H14 2.4400 no . .
O3 H16 2.5393 no . .
O4 H10 2.4847 no . .
O5 H26 2.3962 no . .
O6 H22 2.4250 no . .
N1 H16 2.5911 no . .
N1 H19 2.5655 no . 3_666
N2 H22 2.6129 no . .
N2 H26 2.6115 no . .
C1 H3 2.6390 no . .
C1 H7 2.6276 no . .
C1 H16 3.1923 no . .
C2 H4 3.2605 no . .
C2 H6 3.2499 no . .
C3 H7 3.2316 no . .
C3 H16 3.4649 no . .
C4 H6 3.2385 no . .
C5 H3 3.2147 no . .
C5 H7 3.2160 no . .
C6 H4 3.2416 no . .
C7 H3 3.2326 no . .
C8 H10 2.6690 no . .
C8 H14 2.6449 no . .
C8 H16 3.4853 no . .
C9 H11 3.2776 no . .
C9 H13 3.2680 no . .
C10 H14 3.2402 no . .
C11 H13 3.2509 no . .
C12 H10 3.2229 no . .
C12 H14 3.1981 no . .
C13 H11 3.2524 no . .
C14 H10 3.2473 no . .
C15 H17 3.2686 no . .
C15 H19 3.2792 no . .
C16 H3 3.2938 no . .
C16 H14 3.5904 no . .
C16 H18 3.2325 no . .
C17 H3 3.5885 no . .
C17 H19 3.2347 no . .
C18 H16 3.2358 no . .
C19 H17 3.2314 no . .
C20 H16 3.2864 no . .
C20 H18 3.2740 no . .
C21 H23 3.2275 no . .
C21 H25 3.2158 no . .
C22 H24 3.2447 no . .
C22 H26 3.2452 no . .
C23 H25 3.2342 no . .
C24 H22 3.2541 no . .
C24 H26 3.2453 no . .
C25 H23 3.2300 no . .
C26 H22 3.2439 no . .
C26 H24 3.2436 no . .
H3 H4 2.3846 no . .
H3 H16 2.8380 no . .
H3 H17 3.3719 no . .
H6 H7 2.3623 no . .
H10 H11 2.3956 no . .
H13 H14 2.3423 no . .
H14 H16 3.3665 no . .
H16 H17 2.3022 no . .
H17 H18 2.3120 no . .
H18 H19 2.3102 no . .
H22 H23 2.3570 no . .
H23 H24 2.3064 no . .
H24 H25 2.3123 no . .
H25 H26 2.3680 no . .
F1 H10 2.9547 no . 2_455
F1 H13 3.5527 no . 2_555
F1 H14 3.3344 no . 2_555
F1 H18 3.5912 no . 2_555
F1 H24 2.6287 no . 3_565
F2 H3 3.5973 no . 1_545
F2 H22 3.5409 no . 2_445
F2 H25 3.1132 no . 2_545
F2 H26 3.0555 no . 2_545
O1 H25 3.2012 no . 2_555
O2 H19 2.3145 no . 1_455
O2 H22 3.5411 no . 2_455
O2 H23 3.0449 no . 2_455
O3 H23 2.7821 no . 4_555
O4 H19 2.4426 no . 1_455
O4 H25 2.9765 no . 4_455
O5 H3 3.5778 no . .
O5 H4 3.1856 no . 2_545
O5 H14 3.3299 no . .
O5 H16 2.9083 no . .
O5 H17 2.8253 no . .
O6 H6 3.0391 no . 2_445
O6 H7 3.4237 no . .
O6 H7 3.5761 no . 2_445
O6 H18 2.9821 no . 1_455
O6 H19 2.9967 no . 1_455
N1 H23 3.3802 no . 4_555
N1 H24 3.3225 no . 2_555
N1 H24 3.3781 no . 4_555
N1 H25 3.2877 no . 2_555
C1 H19 3.2295 no . 1_455
C3 H17 3.4507 no . 2_555
C3 H26 3.1728 no . 2_555
C4 H13 3.0711 no . 2_555
C4 H14 3.2383 no . 2_555
C4 H17 3.0997 no . 2_555
C4 H18 3.5316 no . 2_555
C5 H17 3.5504 no . 2_555
C5 H18 3.1395 no . 2_555
C6 H10 3.3721 no . 2_455
C6 H11 3.3495 no . 2_455
C6 H18 3.1246 no . 2_555
C7 H18 3.5147 no . 2_555
C7 H19 3.5325 no . 1_455
C7 H22 2.9774 no . 2_455
C8 H19 3.4251 no . 1_455
C8 H23 3.5239 no . 4_555
C10 H6 2.7666 no . 2_445
C11 H6 2.7838 no . 2_445
C11 H23 3.4402 no . 2_445
C13 H4 2.7799 no . 2_545
C13 H10 3.4822 no . 3_556
C13 H25 3.3749 no . 2_545
C13 H26 3.5194 no . 2_545
C14 H4 2.7699 no . 2_545
C14 H11 3.4524 no . 3_556
C14 H23 3.5576 no . 4_555
C15 H24 2.9523 no . 4_555
C16 H24 3.5020 no . 4_555
C17 H4 3.3682 no . 2_545
C18 H7 3.2528 no . 1_655
C19 H7 3.1220 no . 1_655
C19 H24 3.3840 no . 4_555
C20 H24 2.8916 no . 4_555
C22 H7 3.0629 no . 2_445
C22 H11 3.1342 no . 2_455
C23 H11 2.9582 no . 2_455
C25 H13 2.9377 no . 2_555
C26 H3 3.1125 no . 2_545
C26 H13 2.9691 no . 2_555
H3 F2 3.5973 no . 1_565
H3 O5 3.5778 no . .
H3 C26 3.1125 no . 2_555
H3 H26 2.5410 no . 2_555
H4 O5 3.1856 no . 2_555
H4 C13 2.7799 no . 2_555
H4 C14 2.7699 no . 2_555
H4 C17 3.3682 no . 2_555
H4 H13 2.4274 no . 2_555
H4 H14 2.3598 no . 2_555
H4 H17 3.0820 no . 2_555
H6 O6 3.0391 no . 2_455
H6 C10 2.7666 no . 2_455
H6 C11 2.7838 no . 2_455
H6 H10 2.6062 no . 2_455
H6 H11 2.6520 no . 2_455
H6 H18 3.3792 no . 2_555
H7 O6 3.4237 no . .
H7 O6 3.5761 no . 2_455
H7 C18 3.2528 no . 1_455
H7 C19 3.1220 no . 1_455
H7 C22 3.0629 no . 2_455
H7 H18 3.0817 no . 1_455
H7 H19 2.8628 no . 1_455
H7 H22 2.5835 no . 2_455
H10 F1 2.9547 no . 2_445
H10 C6 3.3721 no . 2_445
H10 C13 3.4822 no . 3_556
H10 H6 2.6062 no . 2_445
H10 H13 3.5147 no . 3_556
H10 H19 3.4918 no . 1_455
H10 H25 2.9679 no . 4_455
H11 C6 3.3495 no . 2_445
H11 C14 3.4524 no . 3_556
H11 C22 3.1342 no . 2_445
H11 C23 2.9582 no . 2_445
H11 H6 2.6520 no . 2_445
H11 H14 3.5672 no . 3_556
H11 H22 2.9248 no . 2_445
H11 H23 2.5829 no . 2_445
H13 F1 3.5527 no . 2_545
H13 C4 3.0711 no . 2_545
H13 C25 2.9377 no . 2_545
H13 C26 2.9691 no . 2_545
H13 H4 2.4274 no . 2_545
H13 H10 3.5147 no . 3_556
H13 H25 2.7448 no . 2_545
H13 H26 2.7850 no . 2_545
H14 F1 3.3344 no . 2_545
H14 O5 3.3299 no . .
H14 C4 3.2383 no . 2_545
H14 H4 2.3598 no . 2_545
H14 H11 3.5672 no . 3_556
H14 H23 3.0356 no . 4_555
H14 H24 3.3695 no . 4_555
H16 O5 2.9083 no . .
H17 O5 2.8253 no . .
H17 C3 3.4507 no . 2_545
H17 C4 3.0997 no . 2_545
H17 C5 3.5504 no . 2_545
H17 H4 3.0820 no . 2_545
H17 H26 3.0855 no . .
H18 F1 3.5912 no . 2_545
H18 O6 2.9821 no . 1_655
H18 C4 3.5316 no . 2_545
H18 C5 3.1395 no . 2_545
H18 C6 3.1246 no . 2_545
H18 C7 3.5147 no . 2_545
H18 H6 3.3792 no . 2_545
H18 H7 3.0817 no . 1_655
H18 H22 3.2411 no . 1_655
H19 O2 2.3145 no . 1_655
H19 O4 2.4426 no . 1_655
H19 O6 2.9967 no . 1_655
H19 C1 3.2295 no . 1_655
H19 C7 3.5325 no . 1_655
H19 C8 3.4251 no . 1_655
H19 H7 2.8628 no . 1_655
H19 H10 3.4918 no . 1_655
H22 F2 3.5409 no . 2_455
H22 O2 3.5411 no . 2_445
H22 C7 2.9774 no . 2_445
H22 H7 2.5835 no . 2_445
H22 H11 2.9248 no . 2_455
H22 H18 3.2411 no . 1_455
H23 O2 3.0449 no . 2_445
H23 O3 2.7821 no . 4_454
H23 N1 3.3802 no . 4_454
H23 C8 3.5239 no . 4_454
H23 C11 3.4402 no . 2_455
H23 C14 3.5576 no . 4_454
H23 H11 2.5829 no . 2_455
H23 H14 3.0356 no . 4_454
H24 F1 2.6287 no . 3_565
H24 N1 3.3225 no . 2_545
H24 N1 3.3781 no . 4_454
H24 C15 2.9523 no . 4_454
H24 C16 3.5020 no . 4_454
H24 C19 3.3840 no . 4_454
H24 C20 2.8916 no . 4_454
H24 H14 3.3695 no . 4_454
H25 F2 3.1132 no . 2_555
H25 O1 3.2012 no . 2_545
H25 O4 2.9765 no . 4_554
H25 N1 3.2877 no . 2_545
H25 C13 3.3749 no . 2_555
H25 H10 2.9679 no . 4_554
H25 H13 2.7448 no . 2_555
H26 F2 3.0555 no . 2_555
H26 C3 3.1728 no . 2_545
H26 C13 3.5194 no . 2_555
H26 H3 2.5410 no . 2_545
H26 H13 2.7850 no . 2_555
H26 H17 3.0855 no . .
#==============================================================================
#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one
# structure analysis in the CIF.
#==============================================================================
# End of CIF
#==============================================================================