#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:33:06 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178570 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/79/4067949.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_4067949
loop_
_publ_author_name
'Gil-Rubio, Juan'
'Guerrero-Leal, Juan'
'Blaya, María'
'Vicente, José'
'Bautista, Delia'
'Jones, Peter G.'
_publ_section_title
;
 Reactions of Half-Sandwich Ethene Complexes of Rhodium(I) toward
 Iodoperfluorocarbons: Perfluoro-alkylation or -arylation of Coordinated
 Ethene versus Oxidative Addition
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              1287
_journal_paper_doi               10.1021/om2009588
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C32 H38 F18 I2 Rh2'
_chemical_formula_weight         1224.24
_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                 103.877(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.6027(14)
_cell_length_b                   8.1396(8)
_cell_length_c                   16.9438(16)
_cell_measurement_reflns_used    7229
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.38
_cell_measurement_theta_min      2.48
_cell_volume                     1955.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω-scan
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0362
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19522
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    2.533
_exptl_absorpt_correction_T_max  0.7858
_exptl_absorpt_correction_T_min  0.5468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.951
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0626P)²+5.5891P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                3221
_reflns_number_total             3703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2009588_si_002.cif
_cod_data_source_block           mbm485s
_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_sg_symbol_H-M      'P 2(1)/n'
_cod_database_code               4067949
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
Rh1 Rh 0.38804(3) 0.37330(5) 0.00980(3) 0.01497(14) Uani 1 1 d .
I1 I 0.46174(3) 0.67319(4) 0.05584(2) 0.01733(13) Uani 1 1 d .
F1 F 0.5932(3) 0.3203(5) 0.2842(2) 0.0309(9) Uani 1 1 d .
F2 F 0.5436(3) 0.0199(5) 0.2493(3) 0.0396(10) Uani 1 1 d .
F3 F 0.5169(3) 0.0536(6) 0.3669(2) 0.0454(11) Uani 1 1 d .
F4 F 0.4015(3) 0.0491(5) 0.2623(3) 0.0437(11) Uani 1 1 d .
F5 F 0.5427(3) 0.3537(6) 0.4171(3) 0.0507(13) Uani 1 1 d .
F6 F 0.3917(3) 0.3234(5) 0.3607(3) 0.0393(10) Uani 1 1 d .
F7 F 0.4643(4) 0.6337(6) 0.4127(3) 0.0525(13) Uani 1 1 d .
F8 F 0.3829(3) 0.6122(5) 0.2904(3) 0.0421(11) Uani 1 1 d .
F9 F 0.5338(4) 0.6348(5) 0.3136(3) 0.0487(12) Uani 1 1 d .
C1 C 0.2673(4) 0.2170(7) 0.0074(4) 0.0190(12) Uani 1 1 d .
C2 C 0.2961(4) 0.2020(7) -0.0671(4) 0.0186(12) Uani 1 1 d .
C3 C 0.2797(4) 0.3585(7) -0.1096(4) 0.0205(13) Uani 1 1 d .
C4 C 0.2477(4) 0.4684(8) -0.0587(4) 0.0250(14) Uani 1 1 d .
C5 C 0.2430(4) 0.3850(7) 0.0160(4) 0.0224(13) Uani 1 1 d .
C6 C 0.2610(5) 0.0786(8) 0.0633(4) 0.0290(15) Uani 1 1 d .
H6A H 0.1999 0.0236 0.0448 0.044 Uiso 1 1 calc R
H6B H 0.2672 0.1211 0.1184 0.044 Uiso 1 1 calc R
H6C H 0.3119 0.0000 0.0633 0.044 Uiso 1 1 calc R
C7 C 0.3244(4) 0.0472(8) -0.1014(4) 0.0253(14) Uani 1 1 d .
H7A H 0.3591 -0.0226 -0.0572 0.038 Uiso 1 1 calc R
H7B H 0.3648 0.0732 -0.1384 0.038 Uiso 1 1 calc R
H7C H 0.2679 -0.0108 -0.1314 0.038 Uiso 1 1 calc R
C8 C 0.2941(5) 0.3894(9) -0.1928(4) 0.0329(16) Uani 1 1 d .
H8A H 0.2372 0.3574 -0.2337 0.049 Uiso 1 1 calc R
H8B H 0.3479 0.3246 -0.2006 0.049 Uiso 1 1 calc R
H8C H 0.3067 0.5064 -0.1989 0.049 Uiso 1 1 calc R
C9 C 0.2200(5) 0.6432(8) -0.0786(5) 0.0365(19) Uani 1 1 d .
H9A H 0.2524 0.6844 -0.1190 0.055 Uiso 1 1 calc R
H9B H 0.2378 0.7100 -0.0292 0.055 Uiso 1 1 calc R
H9C H 0.1516 0.6497 -0.1007 0.055 Uiso 1 1 calc R
C10 C 0.2015(5) 0.4569(9) 0.0799(5) 0.0335(16) Uani 1 1 d .
H10A H 0.1334 0.4701 0.0587 0.050 Uiso 1 1 calc R
H10B H 0.2303 0.5643 0.0960 0.050 Uiso 1 1 calc R
H10C H 0.2136 0.3837 0.1272 0.050 Uiso 1 1 calc R
C11 C 0.4680(4) 0.2747(7) 0.1201(4) 0.0222(13) Uani 1 1 d .
H11A H 0.4603 0.1539 0.1192 0.027 Uiso 1 1 calc R
H11B H 0.5356 0.2989 0.1250 0.027 Uiso 1 1 calc R
C12 C 0.4389(5) 0.3439(8) 0.1939(4) 0.0241(14) Uani 1 1 d .
H12A H 0.3724 0.3124 0.1900 0.029 Uiso 1 1 calc R
H12B H 0.4412 0.4652 0.1912 0.029 Uiso 1 1 calc R
C13 C 0.4982(5) 0.2891(9) 0.2775(4) 0.0294(15) Uani 1 1 d .
C14 C 0.4893(5) 0.0999(9) 0.2892(4) 0.0341(16) Uani 1 1 d .
C15 C 0.4737(5) 0.3810(10) 0.3482(4) 0.0344(17) Uani 1 1 d .
C16 C 0.4641(6) 0.5701(10) 0.3406(5) 0.0386(18) 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'
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'
I I -0.4742 1.8119 '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_3
C11 Rh1 C2 115.0(2) .
C11 Rh1 C5 108.4(3) .
C2 Rh1 C5 65.0(2) .
C11 Rh1 C1 93.9(2) .
C2 Rh1 C1 38.7(2) .
C5 Rh1 C1 38.7(2) .
C11 Rh1 C4 146.6(3) .
C2 Rh1 C4 63.1(2) .
C5 Rh1 C4 38.6(2) .
C1 Rh1 C4 63.5(2) .
C11 Rh1 C3 153.5(2) .
C2 Rh1 C3 38.5(2) .
C5 Rh1 C3 63.8(2) .
C1 Rh1 C3 63.8(2) .
C4 Rh1 C3 36.3(2) .
C11 Rh1 I1 89.44(17) .
C2 Rh1 I1 155.35(16) .
C5 Rh1 I1 105.94(16) .
C1 Rh1 I1 143.18(16) .
C4 Rh1 I1 95.10(16) .
C3 Rh1 I1 116.89(15) .
C11 Rh1 I1 88.87(17) 3_665
C2 Rh1 I1 96.31(17) 3_665
C5 Rh1 I1 158.43(17) 3_665
C1 Rh1 I1 130.16(16) 3_665
C4 Rh1 I1 124.44(18) 3_665
C3 Rh1 I1 95.00(17) 3_665
I1 Rh1 I1 86.513(18) 3_665
Rh1 I1 Rh1 93.487(18) 3_665
C5 C1 C2 107.8(5) .
C5 C1 C6 127.3(6) .
C2 C1 C6 124.9(5) .
C5 C1 Rh1 69.9(3) .
C2 C1 Rh1 69.9(3) .
C6 C1 Rh1 127.3(4) .
C1 C2 C3 108.3(5) .
C1 C2 C7 125.9(5) .
C3 C2 C7 125.2(6) .
C1 C2 Rh1 71.4(3) .
C3 C2 Rh1 74.7(3) .
C7 C2 Rh1 126.6(4) .
C4 C3 C2 107.2(6) .
C4 C3 C8 128.1(6) .
C2 C3 C8 124.7(6) .
C4 C3 Rh1 71.2(3) .
C2 C3 Rh1 66.8(3) .
C8 C3 Rh1 127.6(4) .
C3 C4 C5 109.3(5) .
C3 C4 C9 125.6(6) .
C5 C4 C9 125.1(6) .
C3 C4 Rh1 72.5(3) .
C5 C4 Rh1 67.3(3) .
C9 C4 Rh1 127.7(4) .
C1 C5 C4 107.1(5) .
C1 C5 C10 127.4(6) .
C4 C5 C10 124.4(6) .
C1 C5 Rh1 71.4(3) .
C4 C5 Rh1 74.0(4) .
C10 C5 Rh1 129.4(4) .
C12 C11 Rh1 112.5(4) .
C11 C12 C13 116.2(5) .
F1 C13 C15 105.3(5) .
F1 C13 C12 110.7(5) .
C15 C13 C12 113.2(6) .
F1 C13 C14 106.4(5) .
C15 C13 C14 109.9(6) .
C12 C13 C14 110.9(6) .
F4 C14 F2 108.6(6) .
F4 C14 F3 106.9(6) .
F2 C14 F3 106.7(5) .
F4 C14 C13 111.6(5) .
F2 C14 C13 109.9(6) .
F3 C14 C13 112.9(6) .
F6 C15 F5 108.0(6) .
F6 C15 C13 109.7(6) .
F5 C15 C13 109.2(6) .
F6 C15 C16 107.0(6) .
F5 C15 C16 105.5(6) .
C13 C15 C16 117.2(6) .
F9 C16 F7 109.4(6) .
F9 C16 F8 108.6(7) .
F7 C16 F8 107.1(6) .
F9 C16 C15 111.3(6) .
F7 C16 C15 109.4(6) .
F8 C16 C15 111.0(6) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C11 2.111(6) .
Rh1 C2 2.146(6) .
Rh1 C5 2.147(6) .
Rh1 C1 2.167(6) .
Rh1 C4 2.237(6) .
Rh1 C3 2.253(6) .
Rh1 I1 2.7060(6) .
Rh1 I1 2.7134(6) 3_665
I1 Rh1 2.7134(6) 3_665
F1 C13 1.388(8) .
F2 C14 1.329(8) .
F3 C14 1.335(8) .
F4 C14 1.320(8) .
F5 C15 1.366(8) .
F6 C15 1.351(8) .
F7 C16 1.326(8) .
F8 C16 1.328(9) .
F9 C16 1.320(9) .
C1 C5 1.428(8) .
C1 C2 1.429(9) .
C1 C6 1.488(9) .
C2 C3 1.455(8) .
C2 C7 1.487(9) .
C3 C4 1.398(9) .
C3 C8 1.497(9) .
C4 C5 1.453(9) .
C4 C9 1.495(8) .
C5 C10 1.481(9) .
C11 C12 1.521(9) .
C12 C13 1.538(9) .
C13 C15 1.526(10) .
C13 C14 1.562(10) .
C15 C16 1.548(11) .
