#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:22:22 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178561 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/69/4066911.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_4066911
loop_
_publ_author_name
'Panthi, Basu D.'
'Gipson, Stephen L.'
'Franken, Andreas'
_publ_section_title
;
 Comparison of the Thermal and Reductive Decarbonylation of a Rhodium
 Trifluoroacetyl Diphosphine Complex
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5890
_journal_paper_doi               10.1021/om1007055
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C31 H32 Cl6 F3 I2 P2 Rh'
_chemical_formula_weight         1092.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/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                 110.587(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7676(5)
_cell_length_b                   22.1871(13)
_cell_length_c                   10.3947(6)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.67
_cell_measurement_theta_min      2.34
_cell_volume                     1892.93(19)
_computing_cell_refinement
;
  Bruker APEX2 (Bruker, 2003)
;
_computing_data_collection
;
  Bruker APEX2 (Bruker, 2003)
;
_computing_data_reduction
;
  Bruker APEX2 (Bruker, 2003)
;
_computing_molecular_graphics
;
  ORTEP3 for Windows (Farrugia, 1997)
  XSeed (Barbour, 2001)
;
_computing_publication_material
;
  enCIFer (CCDC, 2002)
;
_computing_structure_refinement
;
  SHELXS-97 (Sheldrick, 1986)
;
_computing_structure_solution
;
  SHELXS-97 (Sheldrick, 1986)
;
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker-Nonius X8 APEX CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0335
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24456
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    2.628
_exptl_absorpt_correction_T_max  0.8354
_exptl_absorpt_correction_T_min  0.7230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0239
_refine_ls_R_factor_gt           0.0194
_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)+(0.0217P)²+2.0612P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0451
_refine_ls_wR_factor_ref         0.0478
_reflns_number_gt                3197
_reflns_number_total             3561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om1007055_si_001.cif
_cod_data_source_block           AFXXXI129A
_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      P21/m
_cod_database_code               4066911
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -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
I1 I 0.370991(19) 0.334415(7) 0.043258(17) 0.01878(6) Uani 1 1 d .
Rh1 Rh 0.60597(3) 0.2500 0.11389(3) 0.01012(7) Uani 1 2 d S
Cl1 Cl 0.14904(11) 0.47436(4) 0.17914(10) 0.0476(2) Uani 1 1 d .
Cl2 Cl 0.38453(13) 0.42382(5) 0.42736(9) 0.0566(3) Uani 1 1 d .
Cl3 Cl 0.18033(9) 0.31555(4) 0.61165(7) 0.03298(17) Uani 1 1 d .
P1 P 0.79091(7) 0.32451(3) 0.11980(6) 0.01183(13) Uani 1 1 d .
F1 F 0.6033(2) 0.29812(8) 0.35995(15) 0.0314(4) Uani 1 1 d .
F2 F 0.8240(3) 0.2500 0.3930(2) 0.0260(5) Uani 1 2 d S
C1 C 0.6641(4) 0.2500 0.3193(4) 0.0147(7) Uani 1 2 d S
C2 C 1.0051(3) 0.30770(11) 0.2147(2) 0.0149(5) Uani 1 1 d .
H2A H 1.0716 0.3419 0.2032 0.018 Uiso 1 1 calc R
H2B H 1.0209 0.3049 0.3136 0.018 Uiso 1 1 calc R
C3 C 1.0699(4) 0.2500 0.1726(4) 0.0164(7) Uani 1 2 d S
H3A H 1.1903 0.2500 0.2143 0.020 Uiso 1 2 calc SR
H3B H 1.0408 0.2500 0.0715 0.020 Uiso 1 2 calc SR
C4 C 0.3561(4) 0.46897(16) 0.2825(3) 0.0382(8) Uani 1 1 d .
H4A H 0.4178 0.4516 0.2278 0.046 Uiso 1 1 calc R
H4B H 0.3996 0.5098 0.3125 0.046 Uiso 1 1 calc R
C5 C 0.1272(5) 0.2500 0.6834(4) 0.0268(9) Uani 1 2 d S
H5A H 0.1847 0.2500 0.7841 0.032 Uiso 1 2 calc SR
H5B H 0.0086 0.2500 0.6653 0.032 Uiso 1 2 calc SR
C11 C 0.7798(3) 0.33760(11) -0.0566(2) 0.0156(5) Uani 1 1 d .
C12 C 0.6403(4) 0.32417(15) -0.1675(3) 0.0303(7) Uani 1 1 d .
H12 H 0.5474 0.3085 -0.1521 0.036 Uiso 1 1 calc R
C13 C 0.6354(4) 0.33348(16) -0.3014(3) 0.0375(8) Uani 1 1 d .
H13 H 0.5399 0.3236 -0.3768 0.045 Uiso 1 1 calc R
C14 C 0.7690(4) 0.35706(14) -0.3245(3) 0.0285(7) Uani 1 1 d .
H14 H 0.7652 0.3637 -0.4158 0.034 Uiso 1 1 calc R
C15 C 0.9070(3) 0.37087(13) -0.2157(3) 0.0261(6) Uani 1 1 d .
H15 H 0.9987 0.3873 -0.2319 0.031 Uiso 1 1 calc R
C16 C 0.9137(3) 0.36108(13) -0.0821(3) 0.0220(6) Uani 1 1 d .
H16 H 1.0104 0.3705 -0.0074 0.026 Uiso 1 1 calc R
C21 C 0.7710(3) 0.39886(11) 0.1874(2) 0.0140(5) Uani 1 1 d .
C22 C 0.7117(3) 0.44740(12) 0.0998(3) 0.0198(6) Uani 1 1 d .
H22 H 0.6759 0.4418 0.0031 0.024 Uiso 1 1 calc R
C23 C 0.7049(3) 0.50418(13) 0.1536(3) 0.0266(6) Uani 1 1 d .
H23 H 0.6654 0.5374 0.0934 0.032 Uiso 1 1 calc R
C24 C 0.7548(3) 0.51273(13) 0.2932(3) 0.0280(6) Uani 1 1 d .
H24 H 0.7491 0.5517 0.3290 0.034 Uiso 1 1 calc R
C25 C 0.8134(3) 0.46458(13) 0.3821(3) 0.0250(6) Uani 1 1 d .
H25 H 0.8471 0.4704 0.4786 0.030 Uiso 1 1 calc R
C26 C 0.8227(3) 0.40764(12) 0.3291(3) 0.0199(6) Uani 1 1 d .
H26 H 0.8643 0.3747 0.3897 0.024 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'
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
C1 Rh1 P1 93.36(7) . .
C1 Rh1 P1 93.36(7) . 4_565
P1 Rh1 P1 91.84(3) . 4_565
C1 Rh1 I1 99.98(7) . 4_565
P1 Rh1 I1 166.619(19) . 4_565
P1 Rh1 I1 88.391(17) 4_565 4_565
C1 Rh1 I1 99.98(7) . .
P1 Rh1 I1 88.391(17) . .
P1 Rh1 I1 166.619(19) 4_565 .
I1 Rh1 I1 88.319(11) 4_565 .
C11 P1 C21 105.32(11) . .
C11 P1 C2 104.85(11) . .
C21 P1 C2 101.31(11) . .
C11 P1 Rh1 107.42(8) . .
C21 P1 Rh1 119.86(8) . .
C2 P1 Rh1 116.67(8) . .
F1 C1 F1 107.2(3) . 4_565
F1 C1 F2 106.0(2) . .
F1 C1 F2 106.0(2) 4_565 .
F1 C1 Rh1 110.94(18) . .
F1 C1 Rh1 110.94(18) 4_565 .
F2 C1 Rh1 115.4(2) . .
C3 C2 P1 115.63(19) . .
C3 C2 H2A 108.4 . .
P1 C2 H2A 108.4 . .
C3 C2 H2B 108.4 . .
P1 C2 H2B 108.4 . .
H2A C2 H2B 107.4 . .
C2 C3 C2 114.1(3) . 4_565
C2 C3 H3A 108.7 . .
C2 C3 H3A 108.7 4_565 .
C2 C3 H3B 108.7 . .
C2 C3 H3B 108.7 4_565 .
H3A C3 H3B 107.6 . .
Cl2 C4 Cl1 111.61(18) . .
Cl2 C4 H4A 109.3 . .
Cl1 C4 H4A 109.3 . .
Cl2 C4 H4B 109.3 . .
Cl1 C4 H4B 109.3 . .
H4A C4 H4B 108.0 . .
Cl3 C5 Cl3 110.5(2) 4_565 .
Cl3 C5 H5A 109.5 4_565 .
Cl3 C5 H5A 109.5 . .
Cl3 C5 H5B 109.5 4_565 .
Cl3 C5 H5B 109.5 . .
H5A C5 H5B 108.1 . .
C12 C11 C16 118.6(2) . .
C12 C11 P1 121.4(2) . .
C16 C11 P1 120.02(19) . .
C11 C12 C13 120.5(3) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C14 C13 C12 120.0(3) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.0(3) . .
C15 C14 H14 120.0 . .
C13 C14 H14 120.0 . .
C14 C15 C16 120.4(3) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C15 C16 C11 120.5(2) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C22 C21 C26 119.5(2) . .
C22 C21 P1 120.90(19) . .
C26 C21 P1 119.57(19) . .
C21 C22 C23 120.0(2) . .
C21 C22 H22 120.0 . .
C23 C22 H22 120.0 . .
C24 C23 C22 120.5(3) . .
C24 C23 H23 119.7 . .
C22 C23 H23 119.7 . .
C23 C24 C25 120.2(3) . .
C23 C24 H24 119.9 . .
C25 C24 H24 119.9 . .
C24 C25 C26 119.7(3) . .
C24 C25 H25 120.2 . .
C26 C25 H25 120.2 . .
C25 C26 C21 120.2(2) . .
C25 C26 H26 119.9 . .
C21 C26 H26 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Rh1 2.6884(3) .
Rh1 C1 2.014(4) .
Rh1 P1 2.3012(6) .
Rh1 P1 2.3012(6) 4_565
Rh1 I1 2.6884(3) 4_565
Cl1 C4 1.759(3) .
Cl2 C4 1.751(4) .
Cl3 C5 1.770(2) .
P1 C11 1.825(2) .
P1 C21 1.825(2) .
P1 C2 1.827(2) .
F1 C1 1.327(3) .
F2 C1 1.341(4) .
C1 F1 1.327(3) 4_565
C2 C3 1.526(3) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C2 1.526(3) 4_565
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 Cl3 1.770(2) 4_565
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C11 C12 1.387(4) .
C11 C16 1.392(4) .
C12 C13 1.392(4) .
C12 H12 0.9500 .
C13 C14 1.379(4) .
C13 H13 0.9500 .
C14 C15 1.369(4) .
C14 H14 0.9500 .
C15 C16 1.387(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.388(4) .
C21 C26 1.394(3) .
C22 C23 1.388(4) .
C22 H22 0.9500 .
C23 C24 1.373(4) .
C23 H23 0.9500 .
C24 C25 1.387(4) .
C24 H24 0.9500 .
C25 C26 1.392(4) .
C25 H25 0.9500 .
C26 H26 0.9500 .
