#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:10:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179883 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/79/7017910.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7017910
loop_
_publ_author_name
'McCarty, W. Jeffrey'
'Yang, Xiaoping'
'DePue Anderson, Lauren J'
'Jones, Richard A.'
_publ_section_title
;
 Dinuclear Rh(II) pyrazolates as CVD precursors for rhodium thin films.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              173
_journal_page_last               179
_journal_paper_doi               10.1039/c1dt11649e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C20 H4 F24 N8 Rh2, C4 H6 N2'
_chemical_formula_sum            'C24 H10 F24 N10 Rh2'
_chemical_formula_weight         1100.24
_chemical_name_common
;
Di-rhodium(ii)tetrakis (mu-(3,5-
bis(trifluoromethyl)pyrazolate))bis(acetonitrile)
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.56
_cell_angle_beta                 102.23
_cell_angle_gamma                92.58
_cell_formula_units_Z            1
_cell_length_a                   9.359
_cell_length_b                   9.434
_cell_length_c                   10.913
_cell_measurement_reflns_used    9248
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.86
_cell_measurement_theta_min      6.02
_cell_volume                     880.270
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+CCD'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0173
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            25948
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.101
_exptl_absorpt_correction_T_max  0.9369
_exptl_absorpt_correction_T_min  0.8884
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001).
The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             530
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0216P)²+1.1928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0500
_reflns_number_gt                3798
_reflns_number_total             4017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11649e.txt
_cod_data_source_block           shelxl2
_cod_database_code               7017910
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Rh1 Rh 0.558839(14) 0.022150(14) 0.612455(13) 0.01123(5) Uani 1 1 d .
N5 N 0.67303(18) 0.06943(19) 0.81741(16) 0.0192(3) Uani 1 1 d .
F2 F 0.96528(13) 0.00496(13) 0.72739(12) 0.0227(2) Uani 1 1 d .
F5 F 0.70951(13) 0.42988(14) 0.85938(12) 0.0262(3) Uani 1 1 d .
F4 F 0.89430(12) 0.32262(13) 0.80148(12) 0.0231(2) Uani 1 1 d .
F1 F 0.88257(16) -0.22392(15) 0.69128(14) 0.0359(3) Uani 1 1 d .
F6 F 0.86987(15) 0.54880(14) 0.80077(13) 0.0314(3) Uani 1 1 d .
F3 F 1.06607(15) -0.17715(18) 0.61322(14) 0.0388(3) Uani 1 1 d .
F9 F 0.20927(15) 0.28249(18) 0.90410(13) 0.0403(4) Uani 1 1 d .
F11 F 0.60079(14) -0.29614(15) 0.75529(13) 0.0295(3) Uani 1 1 d .
F7 F 0.43902(15) 0.32381(17) 0.90911(13) 0.0367(3) Uani 1 1 d .
F10 F 0.40777(17) -0.20796(18) 0.80953(13) 0.0392(3) Uani 1 1 d .
N4 N 0.43824(17) -0.18829(17) 0.54978(15) 0.0148(3) Uani 1 1 d .
N3 N 0.36364(17) 0.11093(17) 0.62400(15) 0.0150(3) Uani 1 1 d .
F8 F 0.34513(18) 0.10288(16) 0.88611(13) 0.0388(3) Uani 1 1 d .
N2 N 0.62913(16) 0.21387(17) 0.58012(15) 0.0143(3) Uani 1 1 d .
N1 N 0.70465(17) -0.08570(17) 0.50565(15) 0.0146(3) Uani 1 1 d .
C5 C 0.7097(2) 0.3511(2) 0.63041(19) 0.0162(3) Uani 1 1 d .
F12 F 0.40753(18) -0.45007(17) 0.71943(15) 0.0438(4) Uani 1 1 d .
C10 C 0.3992(2) -0.3096(2) 0.57915(19) 0.0177(4) Uani 1 1 d .
C11 C 0.7519(2) 0.1108(2) 0.9207(2) 0.0216(4) Uani 1 1 d .
C2 C 0.8343(2) -0.1419(2) 0.50689(19) 0.0167(3) Uani 1 1 d .
C8 C 0.2765(2) 0.1826(2) 0.70166(19) 0.0173(4) Uani 1 1 d .
C6 C 0.6956(2) 0.4172(2) 0.5324(2) 0.0187(4) Uani 1 1 d .
H6 H 0.7393 0.5112 0.5399 0.022 Uiso 1 1 calc R
C1 C 0.9362(2) -0.1347(2) 0.6339(2) 0.0193(4) Uani 1 1 d .
C4 C 0.7946(2) 0.4132(2) 0.7729(2) 0.0181(4) Uani 1 1 d .
C3 C 0.8514(2) -0.2060(2) 0.3770(2) 0.0193(4) Uani 1 1 d .
H3 H 0.9299 -0.2534 0.3493 0.023 Uiso 1 1 calc R
C9 C 0.4539(2) -0.3152(2) 0.7157(2) 0.0217(4) Uani 1 1 d .
C7 C 0.3186(2) 0.2237(2) 0.8503(2) 0.0215(4) Uani 1 1 d .
C12 C 0.8584(3) 0.1672(4) 1.0508(2) 0.0420(6) Uani 1 1 d .
H12A H 0.9562 0.1751 1.0376 0.063 Uiso 1 1 calc R
H12B H 0.8505 0.0983 1.0975 0.063 Uiso 1 1 calc R
H12C H 0.8383 0.2652 1.1027 0.063 Uiso 1 1 calc R
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N3 Rh1 N4 86.84(6) . .
N3 Rh1 N2 86.47(6) . .
N4 Rh1 N2 152.05(6) . .
N3 Rh1 N1 152.03(6) . .
N4 Rh1 N1 86.52(6) . .
N2 Rh1 N1 86.79(6) . .
N3 Rh1 N5 104.56(6) . .
N4 Rh1 N5 106.05(6) . .
N2 Rh1 N5 101.90(6) . .
N1 Rh1 N5 103.39(6) . .
N3 Rh1 Rh1 76.29(4) . 2_656
N4 Rh1 Rh1 76.18(4) . 2_656
N2 Rh1 Rh1 75.86(4) . 2_656
N1 Rh1 Rh1 75.74(4) . 2_656
N5 Rh1 Rh1 177.60(4) . 2_656
C11 N5 Rh1 167.22(16) . .
C10 N4 N2 108.16(15) . 2_656
C10 N4 Rh1 148.10(13) . .
N2 N4 Rh1 103.72(10) 2_656 .
C8 N3 N1 108.22(15) . 2_656
C8 N3 Rh1 147.86(13) . .
N1 N3 Rh1 103.91(11) 2_656 .
C5 N2 N4 107.94(14) . 2_656
C5 N2 Rh1 147.82(13) . .
N4 N2 Rh1 104.23(10) 2_656 .
C2 N1 N3 107.70(15) . 2_656
C2 N1 Rh1 148.25(13) . .
N3 N1 Rh1 104.05(11) 2_656 .
N2 C5 C6 110.04(16) . .
N2 C5 C4 120.72(16) . .
C6 C5 C4 129.22(17) . .
N4 C10 C6 110.09(16) . 2_656
N4 C10 C9 121.12(17) . .
C6 C10 C9 128.78(17) 2_656 .
N5 C11 C12 177.2(2) . .
N1 C2 C3 110.26(16) . .
N1 C2 C1 121.56(17) . .
C3 C2 C1 128.17(17) . .
N3 C8 C3 110.08(16) . 2_656
N3 C8 C7 121.59(17) . .
C3 C8 C7 128.31(18) 2_656 .
C10 C6 C5 103.76(16) 2_656 .
C10 C6 H6 128.1 2_656 .
C5 C6 H6 128.1 . .
F3 C1 F1 107.58(16) . .
F3 C1 F2 106.40(16) . .
F1 C1 F2 105.55(16) . .
F3 C1 C2 111.03(17) . .
F1 C1 C2 112.65(16) . .
F2 C1 C2 113.21(15) . .
F5 C4 F6 107.67(16) . .
F5 C4 F4 106.15(15) . .
F6 C4 F4 106.75(15) . .
F5 C4 C5 113.07(15) . .
F6 C4 C5 110.81(16) . .
F4 C4 C5 112.03(15) . .
C2 C3 C8 103.74(16) . 2_656
C2 C3 H3 128.1 . .
C8 C3 H3 128.1 2_656 .
F11 C9 F10 106.07(17) . .
F11 C9 F12 106.72(16) . .
F10 C9 F12 107.60(17) . .
F11 C9 C10 112.92(16) . .
F10 C9 C10 112.61(16) . .
F12 C9 C10 110.57(17) . .
F7 C7 F9 107.84(17) . .
F7 C7 F8 106.45(17) . .
F9 C7 F8 106.56(17) . .
F7 C7 C8 113.05(16) . .
F9 C7 C8 110.43(17) . .
F8 C7 C8 112.18(16) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N3 2.0542(15) .
Rh1 N4 2.0603(15) .
Rh1 N2 2.0609(15) .
Rh1 N1 2.0642(15) .
Rh1 N5 2.1494(16) .
Rh1 Rh1 2.3533(3) 2_656
N5 C11 1.138(3) .
F2 C1 1.342(2) .
F5 C4 1.334(2) .
F4 C4 1.351(2) .
F1 C1 1.342(2) .
F6 C4 1.339(2) .
F3 C1 1.337(2) .
F9 C7 1.336(2) .
F11 C9 1.336(2) .
F7 C7 1.329(2) .
F10 C9 1.338(2) .
N4 C10 1.343(2) .
N4 N2 1.358(2) 2_656
N3 C8 1.342(2) .
N3 N1 1.358(2) 2_656
F8 C7 1.340(2) .
N2 C5 1.344(2) .
N2 N4 1.358(2) 2_656
N1 C2 1.345(2) .
N1 N3 1.358(2) 2_656
C5 C6 1.395(3) .
C5 C4 1.489(3) .
F12 C9 1.342(2) .
C10 C6 1.390(3) 2_656
C10 C9 1.489(3) .
C11 C12 1.462(3) .
C2 C3 1.389(3) .
C2 C1 1.485(3) .
C8 C3 1.390(3) 2_656
C8 C7 1.494(3) .
C6 C10 1.390(3) 2_656
C6 H6 0.9300 .
C3 C8 1.390(3) 2_656
C3 H3 0.9300 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
