#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:10:45 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179883 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/79/7017909.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_7017909
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, H4 O2'
_chemical_formula_sum            'C20 H8 F24 N8 O2 Rh2'
_chemical_formula_weight         1054.16
_chemical_name_common
;Di-rhodium(ii) tetrakis (mu-(3,5-
bis(trifluoromethyl)pyrazolate))
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.683(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.2451(11)
_cell_length_b                   18.048(2)
_cell_length_c                   9.3478(11)
_cell_measurement_reflns_used    22309
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_volume                     1515.5(3)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            27098
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_correction_T_min  0.9273
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001).
The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.310
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1012
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+3.4419P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0574
_reflns_number_gt                3152
_reflns_number_total             3456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11649e.txt
_cod_data_source_block           shelxl1
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7017909
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
C1 C 0.2621(3) -0.10006(13) -0.2904(3) 0.0140(5) Uani 1 1 d .
C2 C 0.1029(3) -0.09261(13) -0.2847(2) 0.0115(4) Uani 1 1 d .
C3 C -0.0246(3) -0.11710(14) -0.3855(3) 0.0146(5) Uani 1 1 d .
H3 H -0.0306 -0.1438 -0.4718 0.018 Uiso 1 1 calc R
C4 C 0.2859(3) -0.17638(13) 0.2407(3) 0.0143(5) Uani 1 1 d .
C5 C 0.1236(3) -0.15871(13) 0.1987(2) 0.0117(4) Uani 1 1 d .
C6 C 0.3045(3) 0.10160(15) 0.3840(3) 0.0168(5) Uani 1 1 d .
C7 C 0.1408(3) 0.09207(13) 0.3264(2) 0.0123(4) Uani 1 1 d .
C8 C 0.2813(3) 0.16800(13) -0.1468(3) 0.0125(4) Uani 1 1 d .
C9 C 0.1197(2) 0.15509(12) -0.1562(2) 0.0106(4) Uani 1 1 d .
C10 C -0.0028(3) 0.19759(13) -0.2244(3) 0.0129(4) Uani 1 1 d .
H4 H -0.0035 0.2419 -0.2754 0.016 Uiso 1 1 calc R
F1 F 0.27569(16) -0.14269(9) -0.40341(16) 0.0224(3) Uani 1 1 d .
F2 F 0.32429(16) -0.03430(9) -0.30607(18) 0.0233(3) Uani 1 1 d .
F3 F 0.34657(16) -0.13036(9) -0.16708(16) 0.0218(3) Uani 1 1 d .
F4 F 0.31405(16) -0.23428(8) 0.33229(18) 0.0241(3) Uani 1 1 d .
F5 F 0.34029(17) -0.19268(10) 0.12353(17) 0.0278(4) Uani 1 1 d .
F6 F 0.36774(16) -0.11917(9) 0.30847(18) 0.0231(3) Uani 1 1 d .
F7 F 0.33452(19) 0.14696(14) 0.4985(2) 0.0553(7) Uani 1 1 d .
F8 F 0.37429(18) 0.03769(10) 0.4228(2) 0.0378(5) Uani 1 1 d .
F9 F 0.36986(17) 0.13027(10) 0.28226(18) 0.0276(4) Uani 1 1 d .
F10 F 0.30133(16) 0.22114(8) -0.23927(17) 0.0215(3) Uani 1 1 d .
F11 F 0.35717(17) 0.18758(12) -0.01204(17) 0.0333(4) Uani 1 1 d .
F12 F 0.34834(17) 0.10664(8) -0.1813(2) 0.0276(4) Uani 1 1 d .
N1 N 0.0650(2) -0.05592(10) -0.1740(2) 0.0101(4) Uani 1 1 d .
N2 N 0.0764(2) -0.09685(10) 0.1208(2) 0.0102(4) Uani 1 1 d .
N3 N 0.0867(2) 0.05533(11) 0.2005(2) 0.0105(4) Uani 1 1 d .
N4 N 0.0745(2) 0.09491(10) -0.0939(2) 0.0093(4) Uani 1 1 d .
O1 O 0.38416(19) -0.00544(10) 0.0817(2) 0.0191(4) Uani 1 1 d .
Rh1 Rh 0.130220(17) -0.001291(9) 0.024515(17) 0.00777(6) Uani 1 1 d .
H1 H 0.4121 0.0371 0.0817 0.068 Uiso 1 1 d .
H2 H 0.4318 -0.0137 0.1640 0.074(16) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
F1 C1 F2 107.45(19) . .
F1 C1 F3 107.39(19) . .
F2 C1 F3 106.01(19) . .
F1 C1 C2 111.02(19) . .
F2 C1 C2 112.1(2) . .
F3 C1 C2 112.56(19) . .
N1 C2 C3 110.2(2) . .
N1 C2 C1 120.8(2) . .
C3 C2 C1 129.0(2) . .
C7 C3 C2 103.7(2) 3 .
C7 C3 H3 128.2 3 .
C2 C3 H3 128.2 . .
F4 C4 F5 107.31(19) . .
F4 C4 F6 107.16(19) . .
F5 C4 F6 105.94(19) . .
F4 C4 C5 111.52(19) . .
F5 C4 C5 112.34(19) . .
F6 C4 C5 112.21(19) . .
N2 C5 C10 110.0(2) . 3
N2 C5 C4 119.7(2) . .
C10 C5 C4 130.3(2) 3 .
F7 C6 F8 108.7(2) . .
F7 C6 F9 106.9(2) . .
F8 C6 F9 104.9(2) . .
F7 C6 C7 111.3(2) . .
F8 C6 C7 112.6(2) . .
F9 C6 C7 112.1(2) . .
N3 C7 C3 110.2(2) . 3
N3 C7 C6 120.6(2) . .
C3 C7 C6 129.1(2) 3 .
F10 C8 F11 107.35(19) . .
F10 C8 F12 107.12(18) . .
F11 C8 F12 105.9(2) . .
F10 C8 C9 111.40(19) . .
F11 C8 C9 113.04(19) . .
F12 C8 C9 111.64(19) . .
N4 C9 C10 110.0(2) . .
N4 C9 C8 120.6(2) . .
C10 C9 C8 129.4(2) . .
C5 C10 C9 104.1(2) 3 .
C5 C10 H4 128.0 3 .
C9 C10 H4 128.0 . .
C2 N1 N3 107.93(18) . 3
C2 N1 Rh1 148.82(16) . .
N3 N1 Rh1 103.22(13) 3 .
C5 N2 N4 107.95(18) . 3
C5 N2 Rh1 148.09(16) . .
N4 N2 Rh1 103.95(13) 3 .
C7 N3 N1 108.01(18) . 3
C7 N3 Rh1 147.74(16) . .
N1 N3 Rh1 104.24(13) 3 .
C9 N4 N2 108.03(18) . 3
C9 N4 Rh1 148.26(16) . .
N2 N4 Rh1 103.70(13) 3 .
Rh1 O1 H1 106.22(14) . .
Rh1 O1 H2 121.99(15) . .
H1 O1 H2 94.20(19) . .
N3 Rh1 N4 86.52(7) . .
N3 Rh1 N2 87.33(7) . .
N4 Rh1 N2 152.34(7) . .
N3 Rh1 N1 152.51(7) . .
N4 Rh1 N1 86.38(7) . .
N2 Rh1 N1 86.76(7) . .
N3 Rh1 O1 102.38(7) . .
N4 Rh1 O1 105.45(7) . .
N2 Rh1 O1 102.21(7) . .
N1 Rh1 O1 105.11(7) . .
N3 Rh1 Rh1 76.10(5) . 3
N4 Rh1 Rh1 76.29(5) . 3
N2 Rh1 Rh1 76.05(5) . 3
N1 Rh1 Rh1 76.42(5) . 3
O1 Rh1 Rh1 177.68(5) . 3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 F1 1.337(3) .
C1 F2 1.342(3) .
C1 F3 1.346(3) .
C1 C2 1.491(3) .
C2 N1 1.343(3) .
C2 C3 1.395(3) .
C3 C7 1.394(3) 3
C3 H3 0.9300 .
C4 F4 1.337(3) .
C4 F5 1.342(3) .
C4 F6 1.347(3) .
C4 C5 1.493(3) .
C5 N2 1.348(3) .
C5 C10 1.387(3) 3
C6 F7 1.324(3) .
C6 F8 1.329(3) .
C6 F9 1.345(3) .
C6 C7 1.492(3) .
C7 N3 1.341(3) .
C7 C3 1.394(3) 3
C8 F10 1.333(3) .
C8 F11 1.337(3) .
C8 F12 1.345(3) .
C8 C9 1.494(3) .
C9 N4 1.345(3) .
C9 C10 1.391(3) .
C10 C5 1.387(3) 3
C10 H4 0.9300 .
N1 N3 1.365(3) 3
N1 Rh1 2.0613(19) .
N2 N4 1.359(2) 3
N2 Rh1 2.0600(19) .
N3 N1 1.365(3) 3
N3 Rh1 2.0555(19) .
N4 N2 1.359(2) 3
N4 Rh1 2.0578(18) .
O1 Rh1 2.2824(17) .
O1 H1 0.8100(18) .
O1 H2 0.8049(18) .
Rh1 Rh1 2.3426(4) 3
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 F9 0.8100(18) 2.6156(18) 3.106(3) 120.51(13) .
O1 H2 F6 0.8049(18) 2.4852(16) 2.980(2) 120.97(13) .
O1 H2 F2 0.8049(18) 2.4865(15) 3.083(2) 131.91(13) 3_655
O1 H2 F12 0.8049(18) 2.6108(15) 3.038(2) 114.85(13) 3_655
O1 H1 O1 0.8100(18) 2.7511(18) 2.917(3) 93.63(13) 3_655
