#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/60/4076002.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_4076002
loop_
_publ_author_name
'Norman, David W.'
'McDonald, Robert'
'Stryker, Jeffrey M.'
_publ_section_title
;
 Thermally Stable Chromium(III)η3-Allyl Complexes. Direct Structural
 Comparison of Neutral Chromium(II) and Cationic Chromium(III)η3-Allyl
 Redox Isomers
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4461
_journal_paper_doi               10.1021/om050415z
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C13 H23 Cr O2 P2, F6 P'
_chemical_formula_sum            'C13 H23 Cr F6 O2 P3'
_chemical_formula_weight         470.22
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           59
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ab 2a'
_symmetry_space_group_name_H-M   'P m m n :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.7360(7)
_cell_length_b                   11.0577(7)
_cell_length_c                   8.0243(5)
_cell_measurement_reflns_used    6553
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.36
_cell_measurement_theta_min      2.54
_cell_volume                     952.61(10)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7130
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.54
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_max  0.8752
_exptl_absorpt_correction_T_min  0.6788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1082
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0395P)²+1.2159P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0869
_reflns_number_gt                1029
_reflns_number_total             1082
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            om050415zsi20050525_053205.cif
_cod_data_source_block           9
_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_Hall     'P 2 2ab -1ab'
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               4076002
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, 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
Cr Cr 0.2500 0.2500 0.28168(7) 0.01899(18) Uani 1 4 d S
P1 P 0.2500 0.44242(7) 0.15708(9) 0.0256(2) Uani 1 2 d S
O O 0.0201(2) 0.2500 0.0707(3) 0.0361(5) Uani 1 2 d S
C1 C 0.1083(3) 0.2500 0.1520(3) 0.0246(6) Uani 1 2 d S
C2 C 0.1169(2) 0.5382(2) 0.2041(3) 0.0396(6) Uani 1 1 d .
H2A H 0.0398 0.4935 0.1824 0.047 Uiso 1 1 calc R
H2B H 0.1195 0.6105 0.1336 0.047 Uiso 1 1 calc R
H2C H 0.1197 0.5622 0.3216 0.047 Uiso 1 1 calc R
C3 C 0.2500 0.4385(3) -0.0696(4) 0.0395(8) Uani 1 2 d S
H3A H 0.1802 0.3889 -0.1086 0.047 Uiso 0.50 1 calc PR
H3B H 0.3285 0.4036 -0.1091 0.047 Uiso 0.50 1 calc PR
H3C H 0.2413 0.5209 -0.1130 0.047 Uiso 0.50 1 calc PR
C10 C 0.2500 0.3543(5) 0.5142(6) 0.0179(10) Uiso 0.50 2 d SP
H10 H 0.2500 0.4445 0.5222 0.021 Uiso 0.50 2 calc SPR
C11 C 0.1444(4) 0.2812(3) 0.5124(5) 0.0259(9) Uiso 0.50 1 d P
H11 H 0.0561 0.3096 0.5200 0.031 Uiso 0.50 1 calc PR
C12 C 0.1844(4) 0.1599(5) 0.5094(6) 0.0364(10) Uiso 0.50 1 d P
H12 H 0.1296 0.0869 0.5144 0.044 Uiso 0.50 1 calc PR
P2 P 0.2500 0.7500 0.62970(14) 0.0271(3) Uani 1 4 d S
F1 F 0.2500 0.7500 0.8283(3) 0.0365(6) Uani 1 4 d S
F2 F 0.2500 0.7500 0.4301(3) 0.0440(7) Uani 1 4 d S
F3 F 0.14469(13) 0.64713(12) 0.62878(17) 0.0408(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'
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'
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_1
_geom_angle_site_symmetry_3
C1 Cr C1 111.26(17) 2 .
C1 Cr C10 118.70(8) 2 .
C1 Cr C10 118.70(8) . .
C1 Cr C12 101.82(15) 2 8_655
C1 Cr C12 137.22(14) . 8_655
C10 Cr C12 62.03(16) . 8_655
C1 Cr C12 137.22(14) 2 .
C1 Cr C12 101.82(15) . .
C10 Cr C12 62.03(16) . .
C12 Cr C12 37.4(2) 8_655 .
C1 Cr C11 92.85(13) 2 8_655
C1 Cr C11 154.32(13) . 8_655
C10 Cr C11 36.97(12) . 8_655
C12 Cr C11 37.40(17) 8_655 8_655
C12 Cr C11 62.37(15) . 8_655
C1 Cr C11 154.32(13) 2 .
C1 Cr C11 92.84(13) . .
C10 Cr C11 36.97(12) . .
C12 Cr C11 62.37(15) 8_655 .
C12 Cr C11 37.40(17) . .
C11 Cr C11 62.1(2) 8_655 .
C1 Cr P1 76.11(4) 2 2
C1 Cr P1 76.11(4) . 2
C10 Cr P1 146.89(14) . 2
C12 Cr P1 86.75(13) 8_655 2
C12 Cr P1 86.74(13) . 2
C11 Cr P1 120.02(9) 8_655 2
C11 Cr P1 120.02(9) . 2
C1 Cr P1 76.11(3) 2 .
C1 Cr P1 76.11(4) . .
C10 Cr P1 83.45(13) . .
C12 Cr P1 139.83(13) 8_655 .
C12 Cr P1 139.83(13) . .
C11 Cr P1 102.48(9) 8_655 .
C11 Cr P1 102.48(9) . .
P1 Cr P1 129.66(4) 2 .
C2 P1 C2 103.61(17) . 8_655
C2 P1 C3 102.79(11) . .
C2 P1 C3 102.79(11) 8_655 .
C2 P1 Cr 116.04(9) . .
C2 P1 Cr 116.04(9) 8_655 .
C3 P1 Cr 113.79(12) . .
O C1 Cr 179.8(2) . .
C11 C10 C11 109.1(4) . 8_655
C11 C10 Cr 71.7(2) . .
C11 C10 Cr 71.7(2) 8_655 .
C10 C11 C12 107.7(3) . .
C10 C11 Cr 71.3(2) . .
C12 C11 Cr 71.2(3) . .
C12 C12 C11 107.8(2) 8_655 .
C12 C12 Cr 71.31(12) 8_655 .
C11 C12 Cr 71.4(3) . .
F1 P2 F2 180.000(1) . .
F1 P2 F3 90.27(6) . .
F2 P2 F3 89.73(6) . .
F1 P2 F3 90.26(6) . 8_655
F2 P2 F3 89.74(6) . 8_655
F3 P2 F3 89.65(10) . 8_655
F1 P2 F3 90.26(6) . 7_575
F2 P2 F3 89.74(6) . 7_575
F3 P2 F3 90.34(10) . 7_575
F3 P2 F3 179.47(12) 8_655 7_575
F1 P2 F3 90.26(6) . 2_565
F2 P2 F3 89.74(6) . 2_565
F3 P2 F3 179.47(12) . 2_565
F3 P2 F3 90.34(10) 8_655 2_565
F3 P2 F3 89.66(10) 7_575 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cr C1 1.843(3) 2
Cr C1 1.843(3) .
Cr C10 2.193(5) .
Cr C12 2.197(5) 8_655
Cr C12 2.197(5) .
Cr C11 2.199(4) 8_655
Cr C11 2.199(4) .
Cr P1 2.3509(8) 2
Cr P1 2.3509(8) .
P1 C2 1.818(2) .
P1 C2 1.818(2) 8_655
P1 C3 1.819(3) .
O C1 1.150(4) .
C10 C11 1.393(5) .
C10 C11 1.393(5) 8_655
C11 C12 1.409(6) .
C12 C12 1.408(9) 8_655
P2 F1 1.594(3) .
P2 F2 1.602(3) .
P2 F3 1.6038(13) .
P2 F3 1.6038(13) 8_655
P2 F3 1.6038(13) 7_575
P2 F3 1.6038(13) 2_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C1 Cr P1 C2 177.23(13) 2 .
C1 Cr P1 C2 60.75(12) . .
C10 Cr P1 C2 -61.01(9) . .
C12 Cr P1 C2 -90.8(2) 8_655 .
C12 Cr P1 C2 -31.2(2) . .
C11 Cr P1 C2 -92.90(14) 8_655 .
C11 Cr P1 C2 -29.12(14) . .
P1 Cr P1 C2 118.99(9) 2 .
C1 Cr P1 C2 -60.75(12) 2 8_655
C1 Cr P1 C2 -177.23(13) . 8_655
C10 Cr P1 C2 61.01(9) . 8_655
C12 Cr P1 C2 31.2(2) 8_655 8_655
C12 Cr P1 C2 90.8(2) . 8_655
C11 Cr P1 C2 29.12(14) 8_655 8_655
C11 Cr P1 C2 92.90(14) . 8_655
P1 Cr P1 C2 -118.99(9) 2 8_655
C1 Cr P1 C3 58.24(8) 2 .
C1 Cr P1 C3 -58.24(8) . .
C10 Cr P1 C3 180.0 . .
C12 Cr P1 C3 150.20(19) 8_655 .
C12 Cr P1 C3 -150.20(19) . .
C11 Cr P1 C3 148.11(10) 8_655 .
C11 Cr P1 C3 -148.11(10) . .
P1 Cr P1 C3 0.0 2 .
C1 Cr C1 O 0.00(11) 2 .
C10 Cr C1 O 143.17(16) . .
C12 Cr C1 O -138.1(3) 8_655 .
C12 Cr C1 O -152.39(18) . .
C11 Cr C1 O 158.8(2) 8_655 .
C11 Cr C1 O 170.95(14) . .
P1 Cr C1 O -68.80(9) 2 .
P1 Cr C1 O 68.80(13) . .
C1 Cr C10 C11 -168.84(18) 2 .
C1 Cr C10 C11 50.7(3) . .
C12 Cr C10 C11 -80.3(3) 8_655 .
C12 Cr C10 C11 -37.8(2) . .
C11 Cr C10 C11 -118.1(4) 8_655 .
P1 Cr C10 C11 -59.1(2) 2 .
P1 Cr C10 C11 120.9(2) . .
C1 Cr C10 C11 -50.7(3) 2 8_655
C1 Cr C10 C11 168.84(18) . 8_655
C12 Cr C10 C11 37.8(2) 8_655 8_655
C12 Cr C10 C11 80.3(3) . 8_655
C11 Cr C10 C11 118.1(4) . 8_655
P1 Cr C10 C11 59.1(2) 2 8_655
P1 Cr C10 C11 -120.9(2) . 8_655
C11 C10 C11 C12 -0.1(6) 8_655 .
Cr C10 C11 C12 62.3(3) . .
C11 C10 C11 Cr -62.4(3) 8_655 .
C1 Cr C11 C10 23.1(4) 2 .
C1 Cr C11 C10 -137.2(2) . .
C12 Cr C11 C10 79.4(3) 8_655 .
C12 Cr C11 C10 117.0(3) . .
C11 Cr C11 C10 36.9(2) 8_655 .
P1 Cr C11 C10 147.2(2) 2 .
P1 Cr C11 C10 -60.8(2) . .
C1 Cr C11 C12 -93.9(3) 2 .
C1 Cr C11 C12 105.8(2) . .
C10 Cr C11 C12 -117.0(3) . .
C12 Cr C11 C12 -37.6(3) 8_655 .
C11 Cr C11 C12 -80.1(3) 8_655 .
P1 Cr C11 C12 30.2(3) 2 .
P1 Cr C11 C12 -177.8(2) . .
C10 C11 C12 C12 0.0(3) . 8_655
Cr C11 C12 C12 62.40(11) . 8_655
C10 C11 C12 Cr -62.4(3) . .
C1 Cr C12 C12 23.45(13) 2 8_655
C1 Cr C12 C12 163.97(8) . 8_655
C10 Cr C12 C12 -79.65(10) . 8_655
C11 Cr C12 C12 -37.64(17) 8_655 8_655
C11 Cr C12 C12 -117.0(2) . 8_655
P1 Cr C12 C12 88.90(4) 2 8_655
P1 Cr C12 C12 -113.63(17) . 8_655
C1 Cr C12 C11 140.5(2) 2 .
C1 Cr C12 C11 -79.0(2) . .
C10 Cr C12 C11 37.4(2) . .
C12 Cr C12 C11 117.0(2) 8_655 .
C11 Cr C12 C11 79.4(3) 8_655 .
P1 Cr C12 C11 -154.1(2) 2 .
P1 Cr C12 C11 3.4(4) . .
