#------------------------------------------------------------------------------
#$Date: 2009-11-23 07:50:56 +0200 (Mon, 23 Nov 2009) $
#$Revision: 903 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/7102713.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_7102713
loop_
_publ_author_name
'K\"undig, E Peter'
'Lomberget, Thierry'
'Bragg, Ryan'
'Poulard, Cyril'
'Bernardinelli, G\'erald'
_publ_section_title
;
 Desymmetrization of a meso-diol complex derived from
 [Cr(CO)3(eta6-5,8-naphthoquinone)]: use of new diamine acylation
 catalysts.
;
_journal_issue                   13
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1548
_journal_page_last               1549
_journal_year                    2004
_chemical_formula_moiety         'C13 H6 Cr O5'
_chemical_formula_sum            'C13 H6 Cr O5'
_chemical_formula_weight         294.2
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.0.1
_audit_creation_date             2003-09-25
_audit_creation_method           from_xtal_archive_file_using_CIFIO
_audit_update_record             2004-03-12
_cell_angle_alpha                87.055(15)
_cell_angle_beta                 73.479(14)
_cell_angle_gamma                86.175(14)
_cell_formula_units_Z            2
_cell_length_a                   7.1180(8)
_cell_length_b                   7.6777(9)
_cell_length_c                   10.9461(14)
_cell_measurement_reflns_used    5241
_cell_measurement_temperature    200
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      3.03
_cell_volume                     571.90(13)
_computing_cell_refinement       'CELL (Stoe & Cie, 1999)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1999)'
_computing_data_reduction        'XRED (Stoe & Cie, 1999)'
_computing_molecular_graphics    xtal_gx3
_computing_publication_material  xtal_CIFIO
_computing_structure_refinement  xtal_CRYLSQ
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 6
_diffrn_measured_fraction_theta_full .99
_diffrn_measured_fraction_theta_max .99
_diffrn_measurement_device_type  'Stoe Ipds'
_diffrn_measurement_method       \f
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .041
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7602
_diffrn_reflns_theta_full        28.2
_diffrn_reflns_theta_max         28.2
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.013
_exptl_absorpt_correction_T_max  .9436
_exptl_absorpt_correction_T_min  .8447
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'XRED; Stoe & Cie, 1999'
_exptl_crystal_colour            dark-violet
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_meas      not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             296
_exptl_crystal_size_max          .24
_exptl_crystal_size_mid          .14
_exptl_crystal_size_min          .06
_refine_diff_density_max         .574
_refine_diff_density_min         -1.636
_refine_ls_abs_structure_details none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.55(2)
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_number_parameters     190
_refine_ls_number_reflns         1809
_refine_ls_R_factor_gt           .043
_refine_ls_shift/su_max          .00015
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     \w=1/[\s^2^(Fo)+0.00015(Fo^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .041
_reflns_number_gt                1788
_reflns_number_total             2787
_reflns_threshold_expression     'refl observed if Fo > 3.99 \s(Fo)'
_[local]_cod_data_source_file    b404006f.txt
_[local]_cod_data_source_block   LOMBA
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
-x,-y,-z
loop_
_atom_type_symbol
_atom_type_scat_source
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
C Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .002 .002
H Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 0 0
O Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .008 .006
Cr Int._Tables_Vol_IV_Tables_2.2B_and_2.3.1 .284 .624
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
Cr .43152(8) .11420(8) .26603(5) .0273(4) 1.00000 Uani
O1 .2344(4) .3468(4) -.0049(3) .055(3) 1.00000 Uani
O2 .2338(4) .5587(4) .4534(3) .0459(19) 1.00000 Uani
O3 .1682(4) .0747(4) .5341(3) .052(3) 1.00000 Uani
O4 .6154(4) -.2464(4) .2947(3) .050(3) 1.00000 Uani
O5 .1203(4) -.0367(4) .1731(3) .0422(18) 1.00000 Uani
C1 .4061(5) .3994(4) .2718(3) .030(3) 1.00000 Uani
C2 .5625(5) .3407(5) .3232(4) .036(3) 1.00000 Uani
C3 .7146(5) .2309(5) .2531(4) .040(3) 1.00000 Uani
C4 .7162(5) .1795(5) .1300(4) .040(3) 1.00000 Uani
C5 .5662(5) .2390(5) .0779(4) .036(3) 1.00000 Uani
C6 .4073(5) .3477(5) .1493(3) .030(3) 1.00000 Uani
C7 .2395(5) .3993(5) .0977(4) .035(3) 1.00000 Uani
C8 .0817(5) .5143(5) .1743(4) .036(3) 1.00000 Uani
C9 .0802(5) .5642(5) .2892(4) .037(3) 1.00000 Uani
C10 .2379(5) .5103(5) .3481(4) .033(3) 1.00000 Uani
C11 .2699(5) .0888(5) .4317(4) .036(3) 1.00000 Uani
C12 .5448(5) -.1107(5) .2839(4) .037(3) 1.00000 Uani
C13 .2402(5) .0188(5) .2097(4) .033(3) 1.00000 Uani
H2 .553(6) .383(6) .409(4) .05000 1.00000 Uiso
H3 .809(6) .185(6) .298(4) .05000 1.00000 Uiso
H4 .815(6) .107(6) .089(4) .05000 1.00000 Uiso
H5 .555(6) .207(6) .008(5) .05000 1.00000 Uiso
H8 -.026(6) .552(6) .131(4) .05000 1.00000 Uiso
H9 -.019(6) .633(6) .337(4) .05000 1.00000 Uiso
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Cr .0270(3) .0266(3) .0298(3) .00164(17) -.01058(18) -.00231(18)
O1 .0653(17) .067(3) .0370(15) .0211(14) -.0270(13) -.0105(13)
O2 .0460(14) .0510(18) .0428(15) .0003(11) -.0140(11) -.0152(12)
O3 .0552(16) .065(2) .0325(15) -.0098(13) -.0064(12) .0004(12)
O4 .0542(15) .0285(16) .0727(19) .0086(11) -.0281(14) -.0026(13)
O5 .0370(12) .0430(16) .0535(15) -.0039(10) -.0220(11) -.0111(12)
C1 .0312(15) .0225(17) .0369(17) -.0041(12) -.0107(13) .0018(13)
C2 .0341(16) .031(2) .047(2) -.0067(13) -.0195(15) -.0023(15)
C3 .0274(16) .038(3) .056(3) -.0050(13) -.0168(15) .0019(17)
C4 .0272(16) .043(3) .044(3) .0022(14) -.0001(14) .0011(16)
C5 .0378(17) .037(3) .0278(17) .0007(14) -.0036(14) .0016(14)
C6 .0336(15) .0273(18) .0302(16) -.0024(12) -.0101(13) .0058(13)
C7 .0420(17) .033(2) .0312(17) .0005(13) -.0143(14) .0046(14)
C8 .0347(16) .035(2) .0393(19) .0030(13) -.0147(14) .0041(15)
C9 .0348(17) .034(3) .041(2) .0055(14) -.0091(14) -.0011(15)
C10 .0371(16) .0309(19) .0338(18) -.0044(13) -.0124(13) -.0016(14)
C11 .0391(17) .034(3) .040(3) -.0028(14) -.0165(16) -.0037(15)
C12 .0361(17) .035(3) .0429(19) -.0039(14) -.0151(15) -.0049(15)
C13 .0348(17) .0303(19) .0321(17) .0066(13) -.0066(13) -.0021(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cr C1 2.188(4)
Cr C2 2.224(4)
Cr C3 2.224(4)
Cr C4 2.218(3)
Cr C5 2.208(4)
Cr C6 2.174(4)
Cr C11 1.860(4)
Cr C12 1.881(4)
Cr C13 1.851(4)
O1 C7 1.223(5)
O2 C10 1.222(5)
O3 C11 1.153(4)
O4 C12 1.142(5)
O5 C13 1.154(5)
C1 C2 1.422(5)
C1 C6 1.416(5)
C1 C10 1.491(4)
C2 C3 1.394(5)
C2 H2 .99(5)
C3 C4 1.420(6)
C3 H3 .98(5)
C4 C5 1.389(6)
C4 H4 .90(4)
C5 C6 1.423(5)
C5 H5 .84(5)
C6 C7 1.483(5)
C7 C8 1.467(5)
C8 C9 1.330(6)
C8 H8 1.03(5)
C9 C10 1.473(6)
C9 H9 .91(4)
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C11 Cr C12 88.76(15)
C11 Cr C13 88.30(15)
C12 Cr C13 90.08(16)
C2 C1 C6 119.7(3)
C2 C1 C10 120.3(4)
C6 C1 C10 120.0(3)
C1 C2 C3 119.7(4)
C1 C2 H2 115(3)
C3 C2 H2 125(3)
C2 C3 C4 120.5(4)
C2 C3 H3 115(3)
C4 C3 H3 124(3)
C3 C4 C5 120.2(3)
C3 C4 H4 118(4)
C5 C4 H4 122(4)
C4 C5 C6 120.1(4)
C4 C5 H5 124(3)
C6 C5 H5 116(3)
C1 C6 C5 119.7(4)
C1 C6 C7 120.3(3)
C5 C6 C7 119.9(3)
O1 C7 C6 120.6(3)
O1 C7 C8 121.8(4)
C6 C7 C8 117.5(4)
C7 C8 C9 122.4(4)
C7 C8 H8 114(3)
C9 C8 H8 124(3)
C8 C9 C10 122.6(3)
C8 C9 H9 122(4)
C10 C9 H9 115(4)
O2 C10 C1 121.4(4)
O2 C10 C9 121.4(3)
C1 C10 C9 117.2(3)
Cr C11 O3 179.1(4)
Cr C12 O4 179.2(3)
Cr C13 O5 178.3(3)
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 -.8(5)
C6 C1 C2 H2 179(3)
C10 C1 C2 C3 177.2(3)
C10 C1 C2 H2 -3(3)
C2 C1 C6 C5 -.7(5)
C2 C1 C6 C7 176.4(3)
C10 C1 C6 C5 -178.7(3)
C10 C1 C6 C7 -1.6(5)
C2 C1 C10 O2 2.9(5)
C2 C1 C10 C9 -179.2(3)
C6 C1 C10 O2 -179.1(3)
C6 C1 C10 C9 -1.2(5)
C1 C2 C3 C4 1.0(5)
C1 C2 C3 H3 -173(3)
H2 C2 C3 C4 -179(3)
H2 C2 C3 H3 7(4)
C2 C3 C4 C5 .3(6)
C2 C3 C4 H4 -179(3)
H3 C3 C4 C5 174(3)
H3 C3 C4 H4 -5(5)
C3 C4 C5 C6 -1.8(6)
C3 C4 C5 H5 -175(4)
H4 C4 C5 C6 177(4)
H4 C4 C5 H5 4(5)
C4 C5 C6 C1 2.0(5)
C4 C5 C6 C7 -175.1(4)
H5 C5 C6 C1 176(4)
H5 C5 C6 C7 -1(4)
C1 C6 C7 O1 -175.8(4)
C1 C6 C7 C8 4.1(5)
C5 C6 C7 O1 1.3(5)
C5 C6 C7 C8 -178.8(3)
O1 C7 C8 C9 176.1(4)
O1 C7 C8 H8 -4(3)
C6 C7 C8 C9 -3.8(5)
C6 C7 C8 H8 176(3)
C7 C8 C9 C10 .9(6)
C7 C8 C9 H9 -178(4)
H8 C8 C9 C10 -179(3)
H8 C8 C9 H9 1(5)
C8 C9 C10 O2 179.5(4)
C8 C9 C10 C1 1.7(5)
H9 C9 C10 O2 -1(3)
H9 C9 C10 C1 -179(3)