#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:26:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179377 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/74/4327459.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_4327459
loop_
_publ_author_name
'Macarena Poyatos'
'Mercedes Sanaú'
'Eduardo Peris'
_publ_section_title
;
 New Rh(I) and Rh(III) Bisimidazol-2-ylidene Complexes: Synthesis,
 Reactivity, and Molecular Structures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2572
_journal_page_last               2576
_journal_paper_doi               10.1021/ic026212+
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C13 H16 F6 I2 N6 P Rh'
_chemical_formula_weight         758.00
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 120.138(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.607(6)
_cell_length_b                   11.779(4)
_cell_length_c                   11.662(4)
_cell_measurement_temperature    293(2)
_cell_volume                     2448.1(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.1681
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10302
_diffrn_reflns_theta_full        30.53
_diffrn_reflns_theta_max         30.53
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    3.341
_exptl_crystal_density_diffrn    2.057
_exptl_crystal_F_000             1424
_refine_diff_density_max         2.905
_refine_diff_density_min         -1.536
_refine_diff_density_rms         0.271
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.2186
_refine_ls_R_factor_gt           0.0684
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1618P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.3016
_reflns_number_gt                1380
_reflns_number_total             3820
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0262122B_3.cif
_cod_data_source_block           Compound3
_cod_original_cell_volume        2447.9(13)
_cod_database_code               4327459
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.28980(7) 0.5000 0.26866(14) 0.0376(4) Uani 1 2 d S
I1 I 0.19128(8) 0.5000 0.00744(14) 0.0554(5) Uani 1 2 d S
N1 N 0.2100(6) 0.2741(10) 0.2542(11) 0.050(3) Uani 1 1 d .
P1 P 0.0000 0.0000 0.0000 0.0442(17) Uani 1 4 d S
F1 F 0.0778(14) 0.0000 0.094(3) 0.212(14) Uani 1 2 d S
I2 I 0.39455(7) 0.5000 0.52558(13) 0.0502(4) Uani 1 2 d S
P2 P 1.0000 0.5000 0.5000 0.097(4) Uani 1 4 d S
F2 F 0.0000 0.1297(13) 0.0000 0.144(9) Uani 1 2 d S
F3 F -0.013(2) 0.0000 0.116(3) 0.220(15) Uani 1 2 d S
N4 N 0.1973(6) 0.3989(9) 0.3749(10) 0.041(2) Uani 1 1 d .
F4 F 0.9354(10) 0.5796(18) 0.4538(19) 0.213(10) Uani 1 1 d .
N5 N 0.3560(6) 0.3822(9) 0.2415(11) 0.049(3) Uani 1 1 d .
F5 F 0.993(2) 0.5000 0.363(3) 0.221(15) Uani 1 2 d S
C10 C 0.2067(12) 0.5000 0.457(2) 0.054(5) Uani 1 2 d S
C20 C 0.2278(10) 0.2136(13) 0.1625(17) 0.070(5) Uani 1 1 d .
H20A H 0.2394 0.2677 0.1139 0.105 Uiso 1 1 calc R
H20B H 0.1854 0.1689 0.1019 0.105 Uiso 1 1 calc R
H20C H 0.2702 0.1648 0.2123 0.105 Uiso 1 1 calc R
C21 C 0.2295(7) 0.3808(10) 0.2999(14) 0.045(3) Uani 1 1 d .
C24 C 0.1700(9) 0.2253(14) 0.3048(16) 0.062(4) Uani 1 1 d .
H24 H 0.1519 0.1512 0.2896 0.074 Uiso 1 1 calc R
C25 C 0.1612(7) 0.3018(12) 0.3799(15) 0.049(4) Uani 1 1 d .
H25 H 0.1358 0.2919 0.4263 0.059 Uiso 1 1 calc R
C31 C 0.3991(8) 0.3309(12) 0.2370(14) 0.047(3) Uani 1 1 d .
C32 C 0.4573(8) 0.2606(14) 0.2279(17) 0.072(5) Uani 1 1 d .
H32A H 0.4755 0.3013 0.1785 0.108 Uiso 1 1 calc R
H32B H 0.4352 0.1903 0.1839 0.108 Uiso 1 1 calc R
H32C H 0.4982 0.2453 0.3155 0.108 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
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
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
C21 Rh1 C21 87.8(8) . 6_565
C21 Rh1 N5 177.4(5) . 6_565
C21 Rh1 N5 94.2(5) 6_565 6_565
C21 Rh1 N5 94.2(5) . .
C21 Rh1 N5 177.4(5) 6_565 .
N5 Rh1 N5 83.7(6) 6_565 .
C21 Rh1 I2 91.2(4) . .
C21 Rh1 I2 91.2(4) 6_565 .
N5 Rh1 I2 87.0(3) 6_565 .
N5 Rh1 I2 87.0(3) . .
C21 Rh1 I1 91.2(4) . .
C21 Rh1 I1 91.2(4) 6_565 .
N5 Rh1 I1 90.4(3) 6_565 .
N5 Rh1 I1 90.4(3) . .
I2 Rh1 I1 176.59(7) . .
C21 N1 C24 110.4(13) . .
C21 N1 C20 127.2(12) . .
C24 N1 C20 122.3(13) . .
F1 P1 F1 180(4) 5 .
F1 P1 F3 86.6(18) 5 5
F1 P1 F3 93.4(18) . 5
F1 P1 F3 93.4(18) 5 .
F1 P1 F3 86.6(18) . .
F3 P1 F3 180(3) 5 .
F1 P1 F2 90.000(1) 5 5
F1 P1 F2 90.000(1) . 5
F3 P1 F2 90.000(1) 5 5
F3 P1 F2 90.000(1) . 5
F1 P1 F2 90.000(1) 5 .
F1 P1 F2 90.000(1) . .
F3 P1 F2 90.000(1) 5 .
F3 P1 F2 90.000(1) . .
F2 P1 F2 180.0 5 .
F4 P2 F4 78.0(18) 2_756 5_766
F4 P2 F4 180.0(14) 2_756 6_565
F4 P2 F4 102.0(18) 5_766 6_565
F4 P2 F4 102.0(18) 2_756 .
F4 P2 F4 180.000(5) 5_766 .
F4 P2 F4 78.0(18) 6_565 .
F4 P2 F5 88.7(14) 2_756 .
F4 P2 F5 88.7(14) 5_766 .
F4 P2 F5 91.3(14) 6_565 .
F4 P2 F5 91.3(14) . .
F4 P2 F5 91.3(14) 2_756 5_766
F4 P2 F5 91.3(14) 5_766 5_766
F4 P2 F5 88.7(14) 6_565 5_766
F4 P2 F5 88.7(14) . 5_766
F5 P2 F5 180.000(8) . 5_766
C21 N4 C25 110.2(11) . .
C21 N4 C10 126.8(12) . .
C25 N4 C10 122.4(11) . .
C31 N5 Rh1 169.7(11) . .
N4 C10 N4 107.1(16) . 6_565
N1 C21 N4 104.9(11) . .
N1 C21 Rh1 131.7(11) . .
N4 C21 Rh1 123.4(10) . .
C25 C24 N1 108.2(13) . .
C24 C25 N4 106.2(12) . .
N5 C31 C32 178.9(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C21 2.025(12) .
Rh1 C21 2.025(12) 6_565
Rh1 N5 2.079(12) 6_565
Rh1 N5 2.079(12) .
Rh1 I2 2.672(2) .
Rh1 I1 2.682(2) .
N1 C21 1.345(16) .
N1 C24 1.359(17) .
N1 C20 1.476(18) .
P1 F1 1.42(2) 5
P1 F1 1.42(2) .
P1 F3 1.50(2) 5
P1 F3 1.50(2) .
P1 F2 1.528(16) 5
P1 F2 1.528(16) .
P2 F4 1.490(16) 2_756
P2 F4 1.490(16) 5_766
P2 F4 1.490(16) 6_565
P2 F4 1.490(15) .
P2 F5 1.53(2) .
P2 F5 1.53(2) 5_766
N4 C21 1.354(17) .
N4 C25 1.381(15) .
N4 C10 1.482(16) .
N5 C31 1.097(16) .
C10 N4 1.482(15) 6_565
C24 C25 1.33(2) .
C31 C32 1.503(18) .
