#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/42/7204267.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_7204267
loop_
_publ_author_name
'Yen-Ling Tan'
'Andrew J. P. White'
'David A. Widdowson'
'René Wilhelm'
'David J. Williams'
_publ_section_title
;
 Dilithiation of arenetricarbonylchromium(0) complexes with
 enantioselective quench: application to chiral biaryl synthesis
;
_journal_issue                   24
_journal_name_full               'J. Chem. Soc., Perkin Trans. 1'
_journal_page_first              3269
_journal_page_last               3280
_journal_paper_doi               10.1039/b108807f
_journal_year                    2001
_chemical_formula_sum            'C26 H24 Cr O8'
_chemical_formula_weight         516.45
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           144
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31'
_symmetry_space_group_name_H-M   'P 31'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.5356(15)
_cell_length_b                   12.5356(15)
_cell_length_c                   13.273(2)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.38
_cell_measurement_theta_min      1.26
_cell_volume                     1806.3(4)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_sigmaI/netI    0.2220
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2203
_diffrn_reflns_theta_max         63.90
_diffrn_reflns_theta_min         4.07
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.332
_exptl_absorpt_correction_T_max  0.8799
_exptl_absorpt_correction_T_min  0.5995
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.084
_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_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.051
_refine_ls_goodness_of_fit_obs   1.271
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         1741
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.207
_refine_ls_restrained_S_obs      1.269
_refine_ls_R_factor_all          0.1980
_refine_ls_R_factor_obs          0.0879
_refine_ls_shift/esd_max         -0.020
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1789
_refine_ls_wR_factor_obs         0.1245
_reflns_number_observed          1033
_reflns_number_total             2052
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108807f.txt
_cod_data_source_block           DW9904
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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^)+(0.0000P)^2^+0.0000P] 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      P3(1)
_cod_original_formula_sum        'C26 H24 O8 Cr'
_cod_database_code               7204267
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Cr Cr 0.0858(3) 0.3399(3) 0.8209(9) 0.0351(7) Uani 1 d . .
C1 C -0.1274(17) 0.2422(16) 0.8288(15) 0.032(4) Uani 1 d . .
C2 C -0.0688(20) 0.3085(18) 0.9191(19) 0.047(6) Uani 1 d . .
C3 C 0.0166(18) 0.4329(17) 0.9139(17) 0.041(5) Uani 1 d . .
H3A H 0.0502(18) 0.4771(17) 0.9730(17) 0.050 Uiso 1 calc R .
C4 C 0.0535(17) 0.4940(17) 0.8196(18) 0.045(5) Uani 1 d . .
H4A H 0.1111(17) 0.5776(17) 0.8175(18) 0.054 Uiso 1 calc R .
C5 C 0.0055(19) 0.4314(18) 0.7325(18) 0.043(5) Uani 1 d . .
H5A H 0.0293(19) 0.4717(18) 0.6708(18) 0.051 Uiso 1 calc R .
C6 C -0.0802(19) 0.3053(20) 0.7368(16) 0.043(5) Uani 1 d . .
H6A H -0.1072(19) 0.2613(20) 0.6768(16) 0.052 Uiso 1 calc R .
O7 O -0.2171(11) 0.1229(12) 0.8356(12) 0.043(3) Uani 1 d . .
C8 C -0.2760(19) 0.0560(21) 0.7437(16) 0.060(7) Uani 1 d . .
H8A H -0.3472(19) -0.0226(21) 0.7609(16) 0.072 Uiso 1 calc R .
H8B H -0.3042(19) 0.1026(21) 0.7047(16) 0.072 Uiso 1 calc R .
O9 O -0.1973(15) 0.0371(14) 0.6881(14) 0.068(5) Uani 1 d . .
C10 C -0.1696(27) -0.0511(24) 0.7260(20) 0.102(11) Uani 1 d . .
H10A H -0.1130(27) -0.0579(24) 0.6814(20) 0.153 Uiso 1 calc R .
H10B H -0.2439(27) -0.1294(24) 0.7309(20) 0.153 Uiso 1 calc R .
H10C H -0.1330(27) -0.0261(24) 0.7915(20) 0.153 Uiso 1 calc R .
C11 C -0.1146(16) 0.2417(20) 1.0233(16) 0.043(5) Uani 1 d . .
O12 O -0.1224(12) 0.1221(12) 1.0200 0.047(3) Uani 1 d D .
H12 H -0.1375(203) 0.0822(164) 0.9608(76) 0.079(82) Uiso 1 d D .
C13 C -0.2428(15) 0.2231(16) 1.0477(15) 0.034(4) Uani 1 d . .
C14 C -0.2924(19) 0.2861(19) 1.0081(18) 0.052(5) Uani 1 d . .
H14A H -0.2475(19) 0.3451(19) 0.9594(18) 0.062 Uiso 1 calc R .
C15 C -0.4094(16) 0.2686(19) 1.0358(18) 0.051(6) Uani 1 d . .
H15A H -0.4384(16) 0.3174(19) 1.0078(18) 0.062 Uiso 1 calc R .
C16 C -0.4760(22) 0.1827(22) 1.1012(19) 0.062(6) Uani 1 d . .
C17 C -0.4320(19) 0.1147(23) 1.1466(17) 0.066(8) Uani 1 d . .
H17A H -0.4791(19) 0.0562(23) 1.1949(17) 0.079 Uiso 1 calc R .
C18 C -0.3146(23) 0.1335(21) 1.1199(17) 0.064(7) Uani 1 d . .
H18A H -0.2848(23) 0.0867(21) 1.1501(17) 0.076 Uiso 1 calc R .
O19 O -0.5911(14) 0.1506(20) 1.1355(15) 0.094(7) Uani 1 d . .
C20 C -0.6572(24) 0.1949(26) 1.0813(25) 0.106(12) Uani 1 d . .
H20A H -0.7269(24) 0.1845(26) 1.1194(25) 0.159 Uiso 1 d R .
H20B H -0.6850(24) 0.1495(26) 1.0195(25) 0.159 Uiso 1 d R .
H20C H -0.6041(24) 0.2807(26) 1.0666(25) 0.159 Uiso 1 d R .
C21 C -0.0258(17) 0.3046(16) 1.1038(16) 0.035(4) Uani 1 d . .
C22 C -0.0261(20) 0.3988(18) 1.1675(16) 0.048(5) Uani 1 d . .
H22A H -0.0883(20) 0.4181(18) 1.1596(16) 0.058 Uiso 1 calc R .
C23 C 0.0620(16) 0.4590(18) 1.2380(16) 0.046(5) Uani 1 d . .
H23A H 0.0552(16) 0.5142(18) 1.2806(16) 0.055 Uiso 1 calc R .
C24 C 0.1631(19) 0.4411(18) 1.2492(18) 0.046(5) Uani 1 d . .
C25 C 0.1671(17) 0.3538(19) 1.1910(15) 0.041(5) Uani 1 d . .
H25A H 0.2298(17) 0.3355(19) 1.1996(15) 0.049 Uiso 1 calc R .
C26 C 0.0764(15) 0.2923(15) 1.1183(16) 0.035(4) Uani 1 d . .
H26A H 0.0856(15) 0.2383(15) 1.0760(16) 0.042 Uiso 1 calc R .
O27 O 0.2560(14) 0.4985(14) 1.3166(14) 0.070(5) Uani 1 d . .
C28 C 0.2559(25) 0.5823(26) 1.3854(22) 0.106(12) Uani 1 d . .
H28A H 0.2672(25) 0.6551(26) 1.3519(22) 0.159 Uiso 1 d R .
H28B H 0.3220(25) 0.6040(26) 1.4322(22) 0.159 Uiso 1 d R .
H28C H 0.1789(25) 0.5443(26) 1.4210(22) 0.159 Uiso 1 d R .
C29 C 0.0846(17) 0.1978(17) 0.8582(15) 0.036(5) Uani 1 d . .
O29 O 0.0867(16) 0.1100(14) 0.8835(14) 0.075(5) Uani 1 d . .
C30 C 0.2326(18) 0.4250(18) 0.8887(15) 0.044(5) Uani 1 d . .
O30 O 0.3246(14) 0.4740(17) 0.9331(16) 0.087(6) Uani 1 d . .
C31 C 0.1729(20) 0.3481(24) 0.7092(17) 0.060(7) Uani 1 d . .
O31 O 0.2186(16) 0.3454(15) 0.6324(15) 0.078(5) 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 '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
_geom_angle_publ_flag
C31 Cr C29 89.4(10) . . ?
C31 Cr C30 88.2(9) . . ?
C29 Cr C30 87.2(9) . . ?
C31 Cr C3 146.2(10) . . ?
C29 Cr C3 123.9(8) . . ?
C30 Cr C3 87.8(8) . . ?
C31 Cr C4 108.6(10) . . ?
C29 Cr C4 162.0(8) . . ?
C30 Cr C4 93.7(8) . . ?
C3 Cr C4 38.3(7) . . ?
C31 Cr C5 87.3(9) . . ?
C29 Cr C5 149.4(8) . . ?
C30 Cr C5 123.0(8) . . ?
C3 Cr C5 67.1(7) . . ?
C4 Cr C5 36.2(6) . . ?
C31 Cr C6 94.5(8) . . ?
C29 Cr C6 113.3(8) . . ?
C30 Cr C6 159.3(8) . . ?
C3 Cr C6 78.5(7) . . ?
C4 Cr C6 65.9(7) . . ?
C5 Cr C6 37.0(7) . . ?
C31 Cr C2 161.0(9) . . ?
C29 Cr C2 95.0(8) . . ?
C30 Cr C2 110.5(8) . . ?
C3 Cr C2 37.0(7) . . ?
C4 Cr C2 67.8(7) . . ?
C5 Cr C2 79.5(7) . . ?
C6 Cr C2 66.7(8) . . ?
C31 Cr C1 124.7(8) . . ?
C29 Cr C1 91.5(7) . . ?
C30 Cr C1 147.1(7) . . ?
C3 Cr C1 65.8(7) . . ?
C4 Cr C1 77.9(6) . . ?
C5 Cr C1 66.0(7) . . ?
C6 Cr C1 36.3(6) . . ?
C2 Cr C1 36.9(6) . . ?
O7 C1 C6 124.0(16) . . ?
O7 C1 C2 119.2(16) . . ?
C6 C1 C2 116.6(16) . . ?
O7 C1 Cr 133.5(13) . . ?
C6 C1 Cr 67.4(10) . . ?
C2 C1 Cr 67.1(11) . . ?
C3 C2 C1 119.7(19) . . ?
C3 C2 C11 121.1(19) . . ?
C1 C2 C11 118.9(17) . . ?
C3 C2 Cr 69.7(12) . . ?
C1 C2 Cr 76.0(12) . . ?
C11 C2 Cr 132.2(14) . . ?
C2 C3 C4 120.8(18) . . ?
C2 C3 Cr 73.3(12) . . ?
C4 C3 Cr 71.1(12) . . ?
C5 C4 C3 120.6(17) . . ?
C5 C4 Cr 73.6(12) . . ?
C3 C4 Cr 70.6(11) . . ?
C4 C5 C6 119.1(17) . . ?
C4 C5 Cr 70.2(12) . . ?
C6 C5 Cr 71.6(11) . . ?
C5 C6 C1 122.5(16) . . ?
C5 C6 Cr 71.4(11) . . ?
C1 C6 Cr 76.3(10) . . ?
C1 O7 C8 119.0(14) . . ?
O9 C8 O7 110.9(16) . . ?
C8 O9 C10 115.7(18) . . ?
O12 C11 C21 102.7(15) . . ?
O12 C11 C13 108.8(15) . . ?
C21 C11 C13 112.7(16) . . ?
O12 C11 C2 110.0(15) . . ?
C21 C11 C2 112.4(17) . . ?
C13 C11 C2 110.0(15) . . ?
C14 C13 C18 116.0(19) . . ?
C14 C13 C11 126.0(18) . . ?
C18 C13 C11 117.9(17) . . ?
C13 C14 C15 124.0(20) . . ?
C16 C15 C14 118.9(21) . . ?
C15 C16 C17 121.1(23) . . ?
C15 C16 O19 127.4(22) . . ?
C17 C16 O19 111.5(23) . . ?
C16 C17 C18 119.8(21) . . ?
C13 C18 C17 120.1(21) . . ?
C16 O19 C20 117.2(20) . . ?
C26 C21 C22 112.9(16) . . ?
C26 C21 C11 122.9(18) . . ?
C22 C21 C11 123.6(17) . . ?
C23 C22 C21 121.4(18) . . ?
C22 C23 C24 122.4(19) . . ?
C25 C24 O27 115.7(18) . . ?
C25 C24 C23 118.0(20) . . ?
O27 C24 C23 126.2(18) . . ?
C24 C25 C26 119.3(18) . . ?
C21 C26 C25 125.6(17) . . ?
C24 O27 C28 120.6(18) . . ?
O29 C29 Cr 178.0(17) . . ?
O30 C30 Cr 177.0(19) . . ?
O31 C31 Cr 173.5(20) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cr C31 1.81(2) . ?
Cr C29 1.84(2) . ?
Cr C30 1.84(2) . ?
Cr C3 2.16(2) . ?
Cr C4 2.16(2) . ?
Cr C5 2.20(2) . ?
Cr C6 2.21(2) . ?
Cr C2 2.20(2) . ?
Cr C1 2.32(2) . ?
C1 O7 1.35(2) . ?
C1 C6 1.41(2) . ?
C1 C2 1.43(2) . ?
C2 C3 1.38(3) . ?
C2 C11 1.57(3) . ?
C3 C4 1.42(3) . ?
C4 C5 1.36(2) . ?
C5 C6 1.40(3) . ?
O7 C8 1.45(2) . ?
C8 O9 1.34(2) . ?
O9 C10 1.41(3) . ?
C11 O12 1.45(2) . ?
C11 C21 1.46(2) . ?
C11 C13 1.54(2) . ?
C13 C14 1.33(3) . ?
C13 C18 1.41(3) . ?
C14 C15 1.42(3) . ?
C15 C16 1.31(3) . ?
C16 C17 1.36(3) . ?
C16 O19 1.37(3) . ?
C17 C18 1.41(3) . ?
O19 C20 1.40(3) . ?
C21 C26 1.38(2) . ?
C21 C22 1.45(2) . ?
C22 C23 1.35(2) . ?
C23 C24 1.40(2) . ?
C24 C25 1.36(3) . ?
C24 O27 1.36(2) . ?
C25 C26 1.39(2) . ?
O27 C28 1.39(2) . ?
C29 O29 1.16(2) . ?
C30 O30 1.16(2) . ?
C31 O31 1.18(2) . ?
