#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:05:30 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178634 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/45/4074513.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_4074513
loop_
_publ_author_name
'Leung, Chin Hin'
'Incarvito, Christopher D.'
'Crabtree, Robert H.'
_publ_section_title
;
 Interplay of Linker,N-Substituent, and Counterion Effects in the
 Formation and Geometrical Distortion ofN-Heterocyclic Biscarbene
 Complexes of Rhodium(I)
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              6099
_journal_paper_doi               10.1021/om0607189
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C17 H24 F6 N4 O2 P Rh'
_chemical_formula_weight         564.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.66(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.398(3)
_cell_length_b                   12.884(3)
_cell_length_c                   14.925(3)
_cell_measurement_temperature    123(2)
_cell_volume                     2183.7(10)
_computing_cell_refinement       Denzo
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        Denzo
_computing_molecular_graphics    XP
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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    0.0459
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8354
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  0.8734
_exptl_absorpt_correction_T_min  0.8734
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         5382
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0335
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0482P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0849
_reflns_number_gt                4439
_reflns_number_total             5382
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0607189si20060807_014254.cif
_cod_data_source_block           tBu2CO
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2183.5(8)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4074513
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Rh1 Rh 0.698550(15) 0.236799(14) 0.062132(12) 0.01703(7) Uani 1 1 d .
O1 O 0.71823(19) 0.01487(14) 0.13229(14) 0.0416(5) Uani 1 1 d .
O2 O 0.48374(16) 0.19063(15) -0.12281(13) 0.0351(4) Uani 1 1 d .
N1 N 0.93384(17) 0.27312(15) 0.25745(14) 0.0204(4) Uani 1 1 d .
N2 N 0.77447(16) 0.34422(15) 0.25000(13) 0.0178(4) Uani 1 1 d .
N3 N 0.64623(15) 0.44305(14) 0.11634(13) 0.0175(4) Uani 1 1 d .
N4 N 0.67296(15) 0.47403(14) -0.01482(13) 0.0171(4) Uani 1 1 d .
C1 C 0.8189(2) 0.28355(18) 0.19901(16) 0.0188(5) Uani 1 1 d .
C2 C 0.9594(2) 0.32597(18) 0.34456(16) 0.0238(5) Uani 1 1 d .
H2A H 1.0340 0.3292 0.3981 0.029 Uiso 1 1 calc R
C3 C 0.8600(2) 0.37163(18) 0.33988(16) 0.0226(5) Uani 1 1 d .
H3A H 0.8505 0.4140 0.3883 0.027 Uiso 1 1 calc R
C4 C 1.0249(2) 0.2156(2) 0.23348(18) 0.0248(5) Uani 1 1 d .
C5 C 1.0323(3) 0.1056(2) 0.2715(2) 0.0386(7) Uani 1 1 d .
H5A H 1.0543 0.1071 0.3423 0.058 Uiso 1 1 calc R
H5B H 1.0917 0.0669 0.2575 0.058 Uiso 1 1 calc R
H5C H 0.9556 0.0716 0.2393 0.058 Uiso 1 1 calc R
C6 C 0.9905(2) 0.2169(2) 0.12325(19) 0.0344(6) Uani 1 1 d .
H6A H 0.9865 0.2889 0.1008 0.052 Uiso 1 1 calc R
H6B H 0.9134 0.1839 0.0901 0.052 Uiso 1 1 calc R
H6C H 1.0495 0.1789 0.1080 0.052 Uiso 1 1 calc R
C7 C 1.1428(2) 0.2706(2) 0.2833(2) 0.0357(7) Uani 1 1 d .
H7A H 1.1363 0.3418 0.2586 0.054 Uiso 1 1 calc R
H7B H 1.2032 0.2333 0.2692 0.054 Uiso 1 1 calc R
H7C H 1.1650 0.2720 0.3541 0.054 Uiso 1 1 calc R
C8 C 0.65522(18) 0.38562(17) 0.20371(16) 0.0189(5) Uani 1 1 d .
H8A H 0.6389 0.4323 0.2495 0.023 Uiso 1 1 calc R
H8B H 0.5972 0.3283 0.1854 0.023 Uiso 1 1 calc R
C9 C 0.67086(18) 0.39596(17) 0.04514(16) 0.0173(4) Uani 1 1 d .
C10 C 0.64969(19) 0.56836(17) 0.02014(16) 0.0195(5) Uani 1 1 d .
H10A H 0.6460 0.6346 -0.0089 0.023 Uiso 1 1 calc R
C11 C 0.63360(18) 0.54843(17) 0.10171(16) 0.0199(5) Uani 1 1 d .
H11A H 0.6167 0.5975 0.1418 0.024 Uiso 1 1 calc R
C12 C 0.71434(19) 0.47025(18) -0.09637(16) 0.0196(5) Uani 1 1 d .
C13 C 0.7154(2) 0.36012(19) -0.13215(17) 0.0273(5) Uani 1 1 d .
H13A H 0.6352 0.3320 -0.1579 0.041 Uiso 1 1 calc R
H13B H 0.7666 0.3169 -0.0776 0.041 Uiso 1 1 calc R
H13C H 0.7450 0.3604 -0.1839 0.041 Uiso 1 1 calc R
C14 C 0.8393(2) 0.5145(2) -0.05564(18) 0.0281(6) Uani 1 1 d .
H14A H 0.8381 0.5857 -0.0329 0.042 Uiso 1 1 calc R
H14B H 0.8694 0.5147 -0.1071 0.042 Uiso 1 1 calc R
H14C H 0.8903 0.4716 -0.0008 0.042 Uiso 1 1 calc R
C15 C 0.6316(2) 0.53574(19) -0.18078(17) 0.0263(5) Uani 1 1 d .
H15A H 0.5523 0.5058 -0.2054 0.039 Uiso 1 1 calc R
H15B H 0.6598 0.5370 -0.2334 0.039 Uiso 1 1 calc R
H15C H 0.6293 0.6067 -0.1579 0.039 Uiso 1 1 calc R
C16 C 0.7131(2) 0.0960(2) 0.10216(18) 0.0264(5) Uani 1 1 d .
C17 C 0.5658(2) 0.20611(19) -0.05557(17) 0.0228(5) Uani 1 1 d .
P1 P 1.31475(5) 0.12785(5) 0.09358(4) 0.02173(14) Uani 1 1 d .
F1 F 1.42501(15) 0.18409(14) 0.17462(13) 0.0536(5) Uani 1 1 d .
F2 F 1.35948(14) 0.15877(13) 0.01186(12) 0.0416(4) Uani 1 1 d .
F3 F 1.20203(12) 0.07132(12) 0.01392(11) 0.0366(4) Uani 1 1 d .
F4 F 1.26752(15) 0.09714(12) 0.17604(11) 0.0396(4) Uani 1 1 d .
F5 F 1.24070(16) 0.23353(11) 0.07466(13) 0.0385(4) Uani 1 1 d .
F6 F 1.38527(13) 0.02120(12) 0.11280(11) 0.0359(4) Uani 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
C16 Rh1 C17 91.71(11)
C16 Rh1 C1 91.58(10)
C17 Rh1 C1 168.66(9)
C16 Rh1 C9 166.67(9)
C17 Rh1 C9 93.04(9)
C1 Rh1 C9 81.49(9)
C1 N1 C2 110.02(19)
C1 N1 C4 126.45(19)
C2 N1 C4 123.51(19)
C1 N2 C3 111.52(18)
C1 N2 C8 120.58(18)
C3 N2 C8 127.16(19)
C9 N3 C11 111.32(19)
C9 N3 C8 120.63(18)
C11 N3 C8 127.15(19)
C9 N4 C10 109.74(19)
C9 N4 C12 128.04(18)
C10 N4 C12 121.37(18)
N1 C1 N2 104.91(19)
N1 C1 Rh1 139.79(17)
N2 C1 Rh1 115.29(15)
C3 C2 N1 107.9(2)
C2 C3 N2 105.7(2)
N1 C4 C5 108.0(2)
N1 C4 C7 108.6(2)
C5 C4 C7 110.5(2)
N1 C4 C6 109.78(19)
C5 C4 C6 111.3(2)
C7 C4 C6 108.6(2)
N2 C8 N3 107.89(17)
N4 C9 N3 104.77(19)
N4 C9 Rh1 140.18(16)
N3 C9 Rh1 115.00(15)
C11 C10 N4 107.6(2)
C10 C11 N3 106.59(19)
N4 C12 C13 111.71(18)
N4 C12 C15 108.51(18)
C13 C12 C15 108.98(19)
N4 C12 C14 106.68(17)
C13 C12 C14 109.79(19)
C15 C12 C14 111.2(2)
O1 C16 Rh1 173.7(2)
O2 C17 Rh1 176.2(2)
F2 P1 F1 90.65(10)
F2 P1 F6 91.10(9)
F1 P1 F6 90.80(9)
F2 P1 F3 90.78(9)
F1 P1 F3 178.49(10)
F6 P1 F3 89.64(9)
F2 P1 F5 90.20(9)
F1 P1 F5 90.21(10)
F6 P1 F5 178.34(10)
F3 P1 F5 89.32(9)
F2 P1 F4 179.23(9)
F1 P1 F4 89.76(10)
F6 P1 F4 89.54(8)
F3 P1 F4 88.80(9)
F5 P1 F4 89.15(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 C16 1.895(3)
Rh1 C17 1.905(3)
Rh1 C1 2.077(2)
Rh1 C9 2.078(2)
O1 C16 1.130(3)
O2 C17 1.124(3)
N1 C1 1.346(3)
N1 C2 1.387(3)
N1 C4 1.508(3)
N2 C1 1.352(3)
N2 C3 1.381(3)
N2 C8 1.459(3)
N3 C9 1.361(3)
N3 C11 1.374(3)
N3 C8 1.464(3)
N4 C9 1.354(3)
N4 C10 1.398(3)
N4 C12 1.499(3)
C2 C3 1.341(3)
C4 C5 1.517(4)
C4 C7 1.523(3)
C4 C6 1.525(3)
C10 C11 1.335(3)
C12 C13 1.518(3)
C12 C15 1.521(3)
C12 C14 1.529(3)
P1 F2 1.5801(16)
P1 F1 1.5904(17)
P1 F6 1.5916(15)
P1 F3 1.6010(16)
P1 F5 1.6026(16)
P1 F4 1.6101(16)
