#------------------------------------------------------------------------------
#$Date: 2016-03-21 07:18:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178558 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/66/4066605.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_4066605
loop_
_publ_author_name
'Huang, Hui'
'Rheingold, Arnold L.'
'Hughes, Russell P.'
_publ_section_title
;
 Synthesis and X-ray Structure of a Diamagnetic Oxo-Bridged
 Trifluoromethyl−Chromium(V) Complex: Structural and Computational
 Comparisons between CF3and CH3Ligands in Two Different Oxidation States
 of Chromium
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3672
_journal_paper_doi               10.1021/om100543t
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C22 H30 Cr2 F6 O3'
_chemical_formula_weight         560.46
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.910(4)
_cell_length_b                   40.474(10)
_cell_length_c                   8.675(2)
_cell_measurement_reflns_used    6233
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      28.12
_cell_measurement_theta_min      2.81
_cell_volume                     4884(2)
_computing_cell_refinement       'Bruker SMART'
_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      213(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  '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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0470
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8860
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.9627
_exptl_absorpt_correction_T_min  0.7009
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2763
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0600P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                2584
_reflns_number_total             2763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100543t_si_002.cif
_cod_data_source_block           rph351
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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      Fdd2
_cod_database_code               4066605
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
Cr1 Cr -0.22295(3) 0.207672(9) 0.02723(4) 0.02645(12) Uani 1 1 d .
O1 O -0.2500 0.2500 0.0442(3) 0.0272(5) Uani 1 2 d S
O2 O -0.11312(16) 0.20329(5) -0.0203(3) 0.0442(5) Uani 1 1 d .
F1 F -0.13230(17) 0.22522(5) 0.3057(2) 0.0607(5) Uani 1 1 d .
F2 F -0.16857(17) 0.17358(5) 0.3079(2) 0.0605(6) Uani 1 1 d .
F3 F -0.27630(16) 0.21032(5) 0.3546(2) 0.0561(6) Uani 1 1 d .
C1 C -0.2704(2) 0.15605(6) -0.0296(4) 0.0363(6) Uani 1 1 d .
C2 C -0.3422(2) 0.16859(7) 0.0745(3) 0.0372(6) Uani 1 1 d .
C3 C -0.38628(18) 0.19581(6) 0.0029(3) 0.0315(5) Uani 1 1 d .
C4 C -0.34265(19) 0.20044(6) -0.1429(3) 0.0301(5) Uani 1 1 d .
C5 C -0.27160(19) 0.17510(7) -0.1641(3) 0.0333(6) Uani 1 1 d .
C6 C -0.2093(3) 0.12592(7) -0.0036(5) 0.0564(10) Uani 1 1 d .
H6A H -0.2443 0.1064 -0.0363 0.085 Uiso 1 1 calc R
H6B H -0.1938 0.1241 0.1050 0.085 Uiso 1 1 calc R
H6C H -0.1504 0.1278 -0.0629 0.085 Uiso 1 1 calc R
C7 C -0.3746(3) 0.15232(9) 0.2191(4) 0.0575(9) Uani 1 1 d .
H7A H -0.4268 0.1372 0.1962 0.086 Uiso 1 1 calc R
H7B H -0.3966 0.1690 0.2913 0.086 Uiso 1 1 calc R
H7C H -0.3214 0.1402 0.2640 0.086 Uiso 1 1 calc R
C8 C -0.4639(2) 0.21689(9) 0.0716(4) 0.0454(7) Uani 1 1 d .
H8A H -0.5262 0.2074 0.0479 0.068 Uiso 1 1 calc R
H8B H -0.4601 0.2390 0.0287 0.068 Uiso 1 1 calc R
H8C H -0.4557 0.2179 0.1825 0.068 Uiso 1 1 calc R
C9 C -0.3725(2) 0.22550(7) -0.2605(3) 0.0424(7) Uani 1 1 d .
H9A H -0.4255 0.2168 -0.3209 0.064 Uiso 1 1 calc R
H9B H -0.3187 0.2303 -0.3280 0.064 Uiso 1 1 calc R
H9C H -0.3927 0.2456 -0.2089 0.064 Uiso 1 1 calc R
C10 C -0.2117(3) 0.17011(9) -0.3052(4) 0.0519(8) Uani 1 1 d .
H10A H -0.2445 0.1552 -0.3752 0.078 Uiso 1 1 calc R
H10B H -0.1501 0.1607 -0.2763 0.078 Uiso 1 1 calc R
H10C H -0.2014 0.1912 -0.3558 0.078 Uiso 1 1 calc R
C11 C -0.2018(3) 0.20386(7) 0.2601(4) 0.0426(6) 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'
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'
Cr Cr 0.3209 0.6236 '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
O2 Cr1 O1 109.57(8) .
O2 Cr1 C11 96.27(14) .
O1 Cr1 C11 91.24(12) .
O2 Cr1 C5 91.88(10) .
O1 Cr1 C5 125.03(10) .
C11 Cr1 C5 137.31(12) .
O2 Cr1 C4 121.80(11) .
O1 Cr1 C4 91.34(8) .
C11 Cr1 C4 138.22(12) .
C5 Cr1 C4 37.48(10) .
O2 Cr1 C1 96.97(10) .
O1 Cr1 C1 149.44(8) .
C11 Cr1 C1 100.88(12) .
C5 Cr1 C1 36.45(11) .
C4 Cr1 C1 61.08(10) .
O2 Cr1 C2 130.81(11) .
O1 Cr1 C2 119.62(8) .
C11 Cr1 C2 82.95(12) .
C5 Cr1 C2 60.81(10) .
C4 Cr1 C2 59.92(10) .
C1 Cr1 C2 36.63(11) .
O2 Cr1 C3 152.70(10) .
O1 Cr1 C3 89.99(7) .
C11 Cr1 C3 102.33(12) .
C5 Cr1 C3 60.94(9) .
C4 Cr1 C3 35.99(10) .
C1 Cr1 C3 60.16(10) .
C2 Cr1 C3 35.10(10) .
Cr1 O1 Cr1 170.41(16) 14_455
C5 C1 C2 108.7(2) .
C5 C1 C6 125.4(3) .
C2 C1 C6 125.7(3) .
C5 C1 Cr1 70.98(15) .
C2 C1 Cr1 74.83(15) .
C6 C1 Cr1 123.8(2) .
C3 C2 C1 107.6(2) .
C3 C2 C7 126.0(3) .
C1 C2 C7 125.7(3) .
C3 C2 Cr1 72.56(15) .
C1 C2 Cr1 68.55(15) .
C7 C2 Cr1 131.7(2) .
C2 C3 C4 108.2(2) .
C2 C3 C8 125.8(3) .
C4 C3 C8 126.0(3) .
C2 C3 Cr1 72.34(15) .
C4 C3 Cr1 68.65(14) .
C8 C3 Cr1 123.3(2) .
C3 C4 C5 108.3(2) .
C3 C4 C9 125.4(3) .
C5 C4 C9 126.0(3) .
C3 C4 Cr1 75.36(15) .
C5 C4 Cr1 70.54(15) .
C9 C4 Cr1 124.45(19) .
C1 C5 C4 107.2(2) .
C1 C5 C10 127.0(3) .
C4 C5 C10 125.8(3) .
C1 C5 Cr1 72.57(16) .
C4 C5 Cr1 71.98(14) .
C10 C5 Cr1 121.4(2) .
F3 C11 F1 104.3(3) .
F3 C11 F2 104.4(3) .
F1 C11 F2 103.9(3) .
F3 C11 Cr1 118.4(2) .
F1 C11 Cr1 110.0(2) .
F2 C11 Cr1 114.4(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr1 O2 1.592(2) .
Cr1 O1 1.7602(6) .
Cr1 C11 2.047(3) .
Cr1 C5 2.225(3) .
Cr1 C4 2.244(3) .
Cr1 C1 2.246(3) .
Cr1 C2 2.329(3) .
Cr1 C3 2.332(3) .
O1 Cr1 1.7602(6) 14_455
F1 C11 1.356(4) .
F2 C11 1.374(3) .
F3 C11 1.346(4) .
C1 C5 1.399(4) .
C1 C2 1.440(4) .
C1 C6 1.503(4) .
C2 C3 1.405(4) .
C2 C7 1.486(4) .
C3 C4 1.416(4) .
C3 C8 1.500(4) .
C4 C5 1.436(4) .
C4 C9 1.497(4) .
C5 C10 1.495(4) .
