#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:02:37 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180462 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/31/7213153.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_7213153
loop_
_publ_author_name
'Ariffin, Azhar'
'Blake, Alexander J.'
'Ewin, Richard A.'
'Li, Wan-Sheung'
'Simpkins, Nigel S.'
_publ_section_title
;
 The asymmetric synthesis of phosphorus- and sulfur-containing
 tricarbonyl(η6-arene)chromium complexes using the chiral base approach
;
_journal_issue                   21
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 1'
_journal_page_first              3177
_journal_paper_doi               10.1039/a905610f
_journal_year                    1999
_chemical_formula_sum            'C24 H23 Cr O4 P Si'
_chemical_formula_weight         486.48
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   'introduced at calculated postions'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier'
_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                   12.69(2)
_cell_length_b                   12.69(2)
_cell_length_c                   29.55(5)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      12.5
_cell_volume                     4759(13)
_computing_cell_refinement       'STADI4 (Stoe & Cie, 1997a)'
_computing_data_collection       'STADI4 (Stoe & Cie, 1997a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1997b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega/theta
_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  0.1235
_diffrn_reflns_av_sigmaI/netI    0.1199
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            8953
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        'variation +/-8.9'
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.625
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.807
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.68
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.07
_refine_ls_abs_structure_details
'Flack, H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(4)
_refine_ls_extinction_coef       0.00022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4185
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.020P)²+5.09P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1081
_reflns_number_gt                3191
_reflns_number_total             4185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905610fsup1.cif
_cod_data_source_block           (3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.020P)^2^+5.09P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.020P)^2^+5.09P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4(1)2(1)2
_cod_database_code               7213153
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -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_calc_flag
_atom_site_refinement_flags
Cr Cr 0.53072(6) 0.90187(6) 0.12473(3) 0.0215(2) Uani 1 d .
C1 C 0.5415(4) 1.0736(3) 0.11337(15) 0.0180(11) Uani 1 d .
C2 C 0.4418(4) 1.0542(4) 0.13646(17) 0.0212(11) Uani 1 d .
C3 C 0.4487(4) 0.9964(4) 0.17744(18) 0.0265(12) Uani 1 d .
H3 H 0.3870 0.9823 0.1933 0.032 Uiso 1 calc R
C4 C 0.5446(4) 0.9596(4) 0.19510(17) 0.0265(11) Uani 1 d .
H4 H 0.5447 0.9207 0.2218 0.032 Uiso 1 calc R
C5 C 0.6391(4) 0.9805(4) 0.17343(18) 0.0256(12) Uani 1 d .
H5 H 0.7027 0.9576 0.1856 0.031 Uiso 1 calc R
C6 C 0.6361(3) 1.0373(4) 0.13244(17) 0.0218(11) Uani 1 d .
HA H 0.6991 1.0513 0.1175 0.026 Uiso 1 calc R
P P 0.54725(10) 1.14846(10) 0.06099(5) 0.0209(3) Uani 1 d .
O O 0.4552(3) 1.1313(3) 0.03099(11) 0.0269(8) Uani 1 d .
C7 C 0.5626(3) 1.2845(4) 0.07830(15) 0.0219(12) Uani 1 d D
C8 C 0.5971(3) 1.3120(4) 0.12115(18) 0.0269(12) Uani 1 d D
H8 H 0.6150 1.2596 0.1418 0.032 Uiso 1 calc R
C9 C 0.6051(3) 1.4172(4) 0.13363(18) 0.0308(13) Uani 1 d D
H9 H 0.6282 1.4351 0.1625 0.037 Uiso 1 calc R
C10 C 0.5788(3) 1.4947(4) 0.10326(18) 0.0347(15) Uani 1 d D
H10 H 0.5841 1.5652 0.1115 0.042 Uiso 1 calc R
C11 C 0.5447(4) 1.4683(4) 0.0608(2) 0.0392(14) Uani 1 d D
H11 H 0.5271 1.5210 0.0403 0.047 Uiso 1 calc R
C12 C 0.5362(4) 1.3638(4) 0.04824(18) 0.0335(13) Uani 1 d D
H12 H 0.5126 1.3467 0.0194 0.040 Uiso 1 calc R
C13 C 0.6707(4) 1.1109(3) 0.03472(15) 0.0221(11) Uani 1 d D
C14 C 0.7573(4) 1.1784(4) 0.03240(15) 0.0312(13) Uani 1 d D
H14 H 0.7546 1.2438 0.0466 0.037 Uiso 1 calc R
C15 C 0.8461(4) 1.1489(4) 0.00940(15) 0.0325(13) Uani 1 d D
H15 H 0.9035 1.1943 0.0080 0.039 Uiso 1 calc R
C16 C 0.8511(4) 1.0519(4) -0.01186(17) 0.0354(14) Uani 1 d D
H16 H 0.9113 1.0323 -0.0276 0.043 Uiso 1 calc R
C17 C 0.7655(4) 0.9844(4) -0.00941(17) 0.0297(13) Uani 1 d D
H17 H 0.7690 0.9187 -0.0233 0.036 Uiso 1 calc R
C18 C 0.6757(4) 1.0133(4) 0.01331(15) 0.0249(12) Uani 1 d D
H18 H 0.6183 0.9678 0.0144 0.030 Uiso 1 calc R
Si Si 0.30440(10) 1.10595(11) 0.12051(5) 0.0238(3) Uani 1 d .
C19 C 0.3103(4) 1.2512(4) 0.1124(2) 0.0385(16) Uani 1 d .
H19A H 0.2416 1.2770 0.1045 0.058 Uiso 1 calc R
H19B H 0.3589 1.2674 0.0885 0.058 Uiso 1 calc R
H19C H 0.3335 1.2840 0.1399 0.058 Uiso 1 calc R
C20 C 0.2452(4) 1.0368(4) 0.07157(19) 0.0308(13) Uani 1 d .
H20A H 0.1769 1.0659 0.0653 0.046 Uiso 1 calc R
H20B H 0.2383 0.9632 0.0784 0.046 Uiso 1 calc R
H20C H 0.2897 1.0454 0.0455 0.046 Uiso 1 calc R
C21 C 0.2194(4) 1.0811(5) 0.1709(2) 0.0386(15) Uani 1 d .
H21A H 0.1493 1.1058 0.1649 0.058 Uiso 1 calc R
H21B H 0.2476 1.1179 0.1966 0.058 Uiso 1 calc R
H21C H 0.2177 1.0069 0.1772 0.058 Uiso 1 calc R
C22 C 0.6330(4) 0.8239(4) 0.0957(2) 0.0339(14) Uani 1 d .
O22 O 0.6914(3) 0.7722(3) 0.07599(17) 0.0510(13) Uani 1 d .
C23 C 0.4878(4) 0.7771(4) 0.1503(2) 0.0303(13) Uani 1 d .
O23 O 0.4636(3) 0.6987(3) 0.16687(15) 0.0472(11) Uani 1 d .
C24 C 0.4498(4) 0.8682(4) 0.07433(19) 0.0275(12) Uani 1 d .
O24 O 0.4047(3) 0.8409(3) 0.04311(13) 0.0367(9) Uani 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'
Si Si 0.0817 0.0704 '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
C23 Cr C22 86.5(2)
C23 Cr C24 88.2(2)
C22 Cr C24 83.8(3)
C23 Cr C6 144.6(2)
C22 Cr C6 92.3(2)
C24 Cr C6 127.0(2)
C23 Cr C1 158.6(2)
C22 Cr C1 114.5(2)
C24 Cr C1 98.0(2)
C6 Cr C1 37.21(17)
C23 Cr C4 85.5(2)
C22 Cr C4 124.0(2)
C24 Cr C4 150.9(2)
C6 Cr C4 66.02(19)
C1 Cr C4 79.11(18)
C23 Cr C3 92.2(2)
C22 Cr C3 160.9(2)
C24 Cr C3 115.2(2)
C6 Cr C3 77.87(18)
C1 Cr C3 66.64(18)
C4 Cr C3 36.90(19)
C23 Cr C5 107.6(2)
C22 Cr C5 96.1(2)
C24 Cr C5 164.2(2)
C6 Cr C5 37.24(19)
C1 Cr C5 67.54(19)
C4 Cr C5 36.37(19)
C3 Cr C5 66.1(2)
C23 Cr C2 121.6(2)
C22 Cr C2 151.6(2)
C24 Cr C2 92.5(2)
C6 Cr C2 67.59(16)
C1 Cr C2 38.04(17)
C4 Cr C2 67.24(19)
C3 Cr C2 36.82(18)
C5 Cr C2 80.02(17)
C6 C1 C2 119.9(4)
C6 C1 P 118.6(4)
C2 C1 P 121.4(4)
C6 C1 Cr 70.6(2)
C2 C1 Cr 73.0(3)
P C1 Cr 130.3(2)
C3 C2 C1 115.7(4)
C3 C2 Si 116.2(4)
C1 C2 Si 127.9(4)
C3 C2 Cr 70.1(3)
C1 C2 Cr 68.9(2)
Si C2 Cr 134.9(2)
C4 C3 C2 122.9(5)
C4 C3 Cr 71.0(3)
C2 C3 Cr 73.1(3)
C5 C4 C3 121.0(5)
C5 C4 Cr 72.4(3)
C3 C4 Cr 72.0(3)
C4 C5 C6 118.1(5)
C4 C5 Cr 71.2(3)
C6 C5 Cr 70.0(3)
C1 C6 C5 122.4(4)
C1 C6 Cr 72.1(3)
C5 C6 Cr 72.8(3)
O P C7 113.2(2)
O P C13 112.7(2)
C7 P C13 106.17(19)
O P C1 113.7(2)
C7 P C1 105.2(2)
C13 P C1 105.2(2)
C12 C7 C8 118.7(5)
C12 C7 P 119.1(4)
C8 C7 P 122.2(3)
C7 C8 C9 120.5(5)
C10 C9 C8 119.8(5)
C11 C10 C9 120.0(5)
C10 C11 C12 120.4(5)
C11 C12 C7 120.5(5)
C18 C13 C14 119.2(5)
C18 C13 P 117.9(3)
C14 C13 P 122.7(4)
C15 C14 C13 120.3(5)
C14 C15 C16 120.5(5)
C15 C16 C17 119.4(5)
C18 C17 C16 120.7(5)
C17 C18 C13 119.9(5)
C20 Si C19 112.6(3)
C20 Si C21 108.0(3)
C19 Si C21 107.1(3)
C20 Si C2 113.4(2)
C19 Si C2 109.5(2)
C21 Si C2 105.7(3)
O22 C22 Cr 175.5(5)
O23 C23 Cr 178.1(5)
O24 C24 Cr 174.9(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cr C1 2.209(6)
Cr C2 2.265(6)
Cr C3 2.225(6)
Cr C4 2.212(6)
Cr C5 2.226(6)
Cr C6 2.190(6)
Cr C23 1.837(6)
Cr C22 1.843(6)
Cr C24 1.859(6)
C1 C2 1.459(7)
C2 C3 1.418(7)
C3 C4 1.404(7)
C4 C5 1.385(7)
C5 C6 1.410(7)
C1 C6 1.404(7)
C1 P 1.817(5)
P O 1.482(4)
P C7 1.811(6)
P C13 1.812(6)
C7 C12 1.383(6)
C7 C8 1.384(6)
C8 C9 1.389(6)
C9 C10 1.373(6)
C10 C11 1.369(7)
C11 C12 1.381(7)
C13 C18 1.392(6)
C13 C14 1.395(6)
C14 C15 1.369(7)
C15 C16 1.383(6)
C16 C17 1.385(6)
C17 C18 1.373(6)
C2 Si 1.922(6)
Si C20 1.851(6)
Si C19 1.860(6)
Si C21 1.865(6)
C22 O22 1.149(7)
C23 O23 1.150(6)
C24 O24 1.139(6)
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
C6 C1 C2 C3 -1.1(6)
P C1 C2 C3 -178.9(3)
C6 C1 C2 Si 173.9(3)
P C1 C2 Si -3.9(6)
C1 C2 C3 C4 -0.1(7)
Si C2 C3 C4 -175.7(4)
C2 C3 C4 C5 1.5(8)
C3 C4 C5 C6 -1.7(7)
C2 C1 C6 C5 0.9(7)
P C1 C6 C5 178.8(4)
C4 C5 C6 C1 0.5(7)
C6 C1 P O 146.9(3)
C2 C1 P O -35.3(4)
C6 C1 P C7 -88.8(4)
C2 C1 P C7 89.0(4)
C6 C1 P C13 23.1(4)
C2 C1 P C13 -159.1(3)
O P C7 C12 -34.8(4)
C13 P C7 C12 89.3(3)
C1 P C7 C12 -159.5(3)
O P C7 C8 143.2(3)
C13 P C7 C8 -92.6(3)
C1 P C7 C8 18.6(3)
C12 C7 C8 C9 -0.1(2)
P C7 C8 C9 -178.2(3)
C7 C8 C9 C10 -0.1(2)
C8 C9 C10 C11 0.0(5)
C9 C10 C11 C12 0.2(6)
C10 C11 C12 C7 -0.3(6)
C8 C7 C12 C11 0.3(5)
P C7 C12 C11 178.4(4)
O P C13 C18 -47.8(4)
C7 P C13 C18 -172.3(3)
C1 P C13 C18 76.5(3)
O P C13 C14 127.5(3)
C7 P C13 C14 3.1(3)
C1 P C13 C14 -108.1(3)
C18 C13 C14 C15 -0.1(2)
P C13 C14 C15 -175.4(3)
C13 C14 C15 C16 0.1(2)
C14 C15 C16 C17 -0.5(5)
C15 C16 C17 C18 0.9(6)
C16 C17 C18 C13 -0.9(6)
C14 C13 C18 C17 0.5(5)
P C13 C18 C17 176.0(4)
C3 C2 Si C20 -109.3(4)
C1 C2 Si C20 75.8(5)
C3 C2 Si C19 124.0(4)
C1 C2 Si C19 -51.0(5)
C3 C2 Si C21 8.9(4)
C1 C2 Si C21 -166.0(4)
