# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CrCO6_110degree
_database_code_depnum_ccdc_archive 'CCDC 1486566'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            Cr(CO)6_110degree
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Cr O6'
_chemical_formula_sum            'C6 Cr O6'
_chemical_formula_weight         220.06

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   11.5165(3)
_cell_length_b                   10.9267(2)
_cell_length_c                   6.21560(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     782.15(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7640
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      54.20

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.454
_shelx_estimated_absorpt_T_min   0.760
_shelx_estimated_absorpt_T_max   0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            47979
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_av_R_equivalents  0.0640
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.538
_diffrn_reflns_theta_max         54.913
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             5016
_reflns_number_gt                4212
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0531P)²+0.1848P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5016
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.1054
_refine_ls_wR_factor_gt          0.0987
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.37249(2) 0.7500 0.43808(2) 0.00928(3) Uani 1 2 d S T P . .
O1 O 0.51574(9) 0.7500 0.85191(15) 0.02030(14) Uani 1 2 d S T P . .
O2 O 0.53114(6) 0.94643(6) 0.24938(12) 0.01986(10) Uani 1 1 d . . . . .
O3 O 0.22641(9) 0.7500 0.02823(15) 0.02058(14) Uani 1 2 d S T P . .
O4 O 0.21855(6) 0.54973(6) 0.62882(12) 0.02094(10) Uani 1 1 d . . . . .
C1 C 0.46276(8) 0.7500 0.69669(15) 0.01358(11) Uani 1 2 d S T P . .
C2 C 0.47132(6) 0.87316(6) 0.31910(11) 0.01322(8) Uani 1 1 d . . . . .
C3 C 0.28123(8) 0.7500 0.18165(15) 0.01345(11) Uani 1 2 d S T P . .
C4 C 0.27510(6) 0.62501(6) 0.55757(11) 0.01356(8) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.00914(4) 0.00913(4) 0.00958(5) 0.000 0.00005(3) 0.000
O1 0.0202(3) 0.0265(4) 0.0143(3) 0.000 -0.0053(2) 0.000
O2 0.0194(2) 0.0178(2) 0.0224(3) 0.00232(17) 0.00315(17) -0.00690(17)
O3 0.0191(3) 0.0279(4) 0.0147(3) 0.000 -0.0054(2) 0.000
O4 0.0185(2) 0.0186(2) 0.0257(3) 0.00678(18) 0.00201(18) -0.00531(17)
C1 0.0130(3) 0.0153(3) 0.0125(3) 0.000 -0.0009(2) 0.000
C2 0.01304(19) 0.01256(17) 0.0141(2) 0.00030(14) 0.00044(15) -0.00121(14)
C3 0.0128(3) 0.0148(3) 0.0127(3) 0.000 -0.0008(2) 0.000
C4 0.01264(19) 0.01315(18) 0.0149(2) 0.00164(14) 0.00033(15) -0.00076(14)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cr1 C3 1.9092(9) . ?
Cr1 C2 1.9114(6) 7_575 ?
Cr1 C2 1.9114(6) . ?
Cr1 C1 1.9143(9) . ?
Cr1 C4 1.9170(6) . ?
Cr1 C4 1.9170(6) 7_575 ?
O1 C1 1.1415(12) . ?
O2 C2 1.1417(8) . ?
O3 C3 1.1436(12) . ?
O4 C4 1.1387(8) . ?

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
C3 Cr1 C2 90.28(3) . 7_575 ?
C3 Cr1 C2 90.27(3) . . ?
C2 Cr1 C2 89.51(4) 7_575 . ?
C3 Cr1 C1 179.49(4) . . ?
C2 Cr1 C1 90.09(3) 7_575 . ?
C2 Cr1 C1 90.09(3) . . ?
C3 Cr1 C4 90.08(3) . . ?
C2 Cr1 C4 89.81(3) 7_575 . ?
C2 Cr1 C4 179.24(3) . . ?
C1 Cr1 C4 89.57(3) . . ?
C3 Cr1 C4 90.08(3) . 7_575 ?
C2 Cr1 C4 179.24(3) 7_575 7_575 ?
C2 Cr1 C4 89.81(3) . 7_575 ?
C1 Cr1 C4 89.57(3) . 7_575 ?
C4 Cr1 C4 90.87(4) . 7_575 ?
O1 C1 Cr1 179.42(9) . . ?
O2 C2 Cr1 179.36(7) . . ?
O3 C3 Cr1 179.90(9) . . ?
O4 C4 Cr1 179.05(7) . . ?

_refine_diff_density_max         0.723
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.117

_shelxl_version_number           2013-2

_shelx_res_file                  
;
TITL a15_13+14.res in Pnma
CELL  0.71073  11.5165  10.9267   6.2156   90.000   90.000   90.000
ZERR    4.000   0.0003   0.0002   0.0001    0.000    0.000    0.000
LATT  1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, -Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SFAC  C   O   CR
UNIT   24   24   4
TEMP -173
OMIT 4 6 0
ACTA
SIZE 0.20  0.18  0.13
L.S. 10
BOND $H
FMAP 2
PLAN -20
WGHT    0.053100    0.184800
FVAR       0.74237
CR1   3    0.372492    0.750000    0.438080    10.50000    0.00914    0.00913 =
         0.00958    0.00000    0.00005    0.00000
O1    2    0.515742    0.750000    0.851915    10.50000    0.02018    0.02646 =
         0.01427    0.00000   -0.00534    0.00000
O2    2    0.531141    0.946432    0.249385    11.00000    0.01945    0.01775 =
         0.02238    0.00232    0.00315   -0.00690
O3    2    0.226414    0.750000    0.028230    10.50000    0.01909    0.02793 =
         0.01473    0.00000   -0.00537    0.00000
O4    2    0.218553    0.549729    0.628820    11.00000    0.01854    0.01862 =
         0.02566    0.00678    0.00201   -0.00531
C1    1    0.462762    0.750000    0.696691    10.50000    0.01299    0.01526 =
         0.01249    0.00000   -0.00093    0.00000
C2    1    0.471316    0.873164    0.319102    11.00000    0.01304    0.01256 =
         0.01407    0.00030    0.00044   -0.00121
C3    1    0.281229    0.750000    0.181654    10.50000    0.01281    0.01485 =
         0.01271    0.00000   -0.00081    0.00000
C4    1    0.275099    0.625005    0.557569    11.00000    0.01264    0.01315 =
         0.01491    0.00164    0.00033   -0.00076
HKLF 4

REM  a15_13+14.res in Pnma
REM R1 =  0.0360 for    4212 Fo > 4sig(Fo)  and  0.0448 for all    5016 data
REM     67 parameters refined using      0 restraints

END

WGHT      0.0401      0.2556

REM Highest difference peak  0.723,  deepest hole -1.613,  1-sigma level  0.117
Q1    1   0.5014  0.9146  0.2962  11.00000  0.05    0.72
Q2    1   0.4323  0.8304  0.3449  11.00000  0.05    0.71
Q3    1   0.3090  0.8350  0.5230  11.00000  0.05    0.68
Q4    1   0.2484  0.7500  0.1069  10.50000  0.05    0.59
Q5    1   0.2475  0.5928  0.6215  11.00000  0.05    0.59
Q6    1   0.3755  0.7500  0.1932  10.50000  0.05    0.54
Q7    1   0.3014  0.7500  0.2709  10.50000  0.05    0.53
Q8    1   0.3615  0.8221  0.4275  11.00000  0.05    0.46
Q9    1   0.4404  0.7500  0.4660  10.50000  0.05    0.46
Q10   1   0.4026  0.8113  0.4454  11.00000  0.05    0.46
Q11   1   0.4698  0.7500  0.7931  10.50000  0.05    0.46
Q12   1   0.4329  0.7793  0.5974  11.00000  0.05    0.44
Q13   1   0.3787  0.8194  0.4715  11.00000  0.05    0.43
Q14   1   0.4376  0.8231  0.5195  11.00000  0.05    0.42
Q15   1   0.3726  0.7892  0.5403  11.00000  0.05    0.42
Q16   1   0.4393  0.7500  0.2599  10.50000  0.05    0.42
Q17   1   0.3787  0.7500  0.3068  10.50000  0.05    0.39
Q18   1   0.3297  0.8559  0.4354  11.00000  0.05    0.38
Q19   1   0.3997  0.7500  0.6243  10.50000  0.05    0.37
Q20   1   0.4745  0.8437  0.5018  11.00000  0.05    0.37
;
_shelx_res_checksum              5063
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_CrCO6_90degree
_database_code_depnum_ccdc_archive 'CCDC 1486567'
_audit_update_record             
;
2016-06-17 deposited with the CCDC.
2016-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            Cr(CO)6_90degree
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Cr O6'
_chemical_formula_sum            'C6 Cr O6'
_chemical_formula_weight         220.06

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'
O O 0.0106 0.0060 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'

_cell_length_a                   11.5165(3)
_cell_length_b                   10.9267(2)
_cell_length_c                   6.21560(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     782.15(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7640
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      54.20

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.869
_exptl_crystal_F_000             432
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_absorpt_coefficient_mu    1.454
_shelx_estimated_absorpt_T_min   0.760
_shelx_estimated_absorpt_T_max   0.833
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5759
_exptl_absorpt_correction_T_max  0.7507
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Incoatec microsource'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            35569
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.538
_diffrn_reflns_theta_max         44.991
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             3287
_reflns_number_gt                2932
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0371P)²+0.2335P]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    undef
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3287
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0283
_refine_ls_wR_factor_ref         0.0788
_refine_ls_wR_factor_gt          0.0758
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.37248(2) 0.7500 0.43809(2) 0.00852(3) Uani 1 2 d S T P . .
O1 O 0.51576(8) 0.7500 0.85197(15) 0.01960(14) Uani 1 2 d S T P . .
O2 O 0.53120(6) 0.94647(6) 0.24933(12) 0.01916(10) Uani 1 1 d . . . . .
O3 O 0.22641(8) 0.7500 0.02816(15) 0.01985(14) Uani 1 2 d S T P . .
O4 O 0.21855(6) 0.54971(6) 0.62894(12) 0.02030(11) Uani 1 1 d . . . . .
C1 C 0.46277(8) 0.7500 0.69677(16) 0.01293(12) Uani 1 2 d S T P . .
C2 C 0.47132(6) 0.87315(6) 0.31909(11) 0.01254(9) Uani 1 1 d . . . . .
C3 C 0.28128(8) 0.7500 0.18154(16) 0.01272(12) Uani 1 2 d S T P . .
C4 C 0.27513(6) 0.62502(6) 0.55752(11) 0.01293(9) Uani 1 1 d . . . . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cr1 0.00820(5) 0.00836(5) 0.00900(5) 0.000 0.00005(3) 0.000
O1 0.0193(3) 0.0257(4) 0.0138(3) 0.000 -0.0051(2) 0.000
O2 0.0185(2) 0.0172(2) 0.0218(3) 0.00222(18) 0.00297(18) -0.00656(18)
O3 0.0180(3) 0.0271(4) 0.0145(3) 0.000 -0.0049(2) 0.000
O4 0.0178(2) 0.0179(2) 0.0252(3) 0.00657(19) 0.00192(19) -0.00513(18)
C1 0.0123(3) 0.0145(3) 0.0120(3) 0.000 -0.0008(2) 0.000
C2 0.0122(2) 0.01197(19) 0.0135(2) 0.00036(16) 0.00041(16) -0.00102(16)
C3 0.0119(3) 0.0140(3) 0.0123(3) 0.000 -0.0008(2) 0.000
C4 0.0120(2) 0.0124(2) 0.0144(2) 0.00161(16) 0.00031(16) -0.00083(16)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Cr1 C3 1.9094(10) . ?
Cr1 C2 1.9113(7) 7_575 ?
Cr1 C2 1.9114(7) . ?
Cr1 C1 1.9148(10) . ?
Cr1 C4 1.9165(7) . ?
Cr1 C4 1.9165(7) 7_575 ?
O1 C1 1.1415(13) . ?
O2 C2 1.1425(9) . ?
O3 C3 1.1437(13) . ?
O4 C4 1.1396(9) . ?

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
C3 Cr1 C2 90.25(3) . 7_575 ?
C3 Cr1 C2 90.25(3) . . ?
C2 Cr1 C2 89.50(4) 7_575 . ?
C3 Cr1 C1 179.52(4) . . ?
C2 Cr1 C1 90.09(3) 7_575 . ?
C2 Cr1 C1 90.09(3) . . ?
C3 Cr1 C4 90.10(3) . . ?
C2 Cr1 C4 89.80(3) 7_575 . ?
C2 Cr1 C4 179.22(3) . . ?
C1 Cr1 C4 89.56(3) . . ?
C3 Cr1 C4 90.10(3) . 7_575 ?
C2 Cr1 C4 179.22(3) 7_575 7_575 ?
C2 Cr1 C4 89.80(3) . 7_575 ?
C1 Cr1 C4 89.56(3) . 7_575 ?
C4 Cr1 C4 90.89(4) . 7_575 ?
O1 C1 Cr1 179.43(9) . . ?
O2 C2 Cr1 179.35(7) . . ?
O3 C3 Cr1 179.84(9) . . ?
O4 C4 Cr1 179.06(7) . . ?

_refine_diff_density_max         0.711
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-2

_shelx_res_file                  
;
TITL a15_13+14.res in Pnma
CELL  0.71073  11.5165  10.9267   6.2156   90.000   90.000   90.000
ZERR    4.000   0.0003   0.0002   0.0001    0.000    0.000    0.000
LATT  1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, -Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SFAC  C   O   CR
UNIT   24   24   4
TEMP -173
OMIT 4 6 0
ACTA
OMIT -2 90
SIZE 0.20  0.18  0.13
L.S. 10
BOND $H
FMAP 2
PLAN -20
WGHT    0.037100    0.233500
FVAR       0.72379
CR1   3    0.372484    0.750000    0.438086    10.50000    0.00820    0.00836 =
         0.00900    0.00000    0.00005    0.00000
O1    2    0.515760    0.750000    0.851973    10.50000    0.01931    0.02565 =
         0.01384    0.00000   -0.00508    0.00000
O2    2    0.531200    0.946466    0.249327    11.00000    0.01849    0.01722 =
         0.02178    0.00222    0.00297   -0.00656
O3    2    0.226409    0.750000    0.028162    10.50000    0.01796    0.02714 =
         0.01447    0.00000   -0.00491    0.00000
O4    2    0.218555    0.549709    0.628944    11.00000    0.01780    0.01792 =
         0.02517    0.00657    0.00192   -0.00513
C1    1    0.462770    0.750000    0.696773    10.50000    0.01227    0.01449 =
         0.01203    0.00000   -0.00082    0.00000
C2    1    0.471317    0.873152    0.319093    11.00000    0.01216    0.01197 =
         0.01349    0.00036    0.00041   -0.00102
C3    1    0.281278    0.750000    0.181541    10.50000    0.01192    0.01398 =
         0.01225    0.00000   -0.00076    0.00000
C4    1    0.275135    0.625016    0.557519    11.00000    0.01196    0.01243 =
         0.01441    0.00161    0.00031   -0.00083
HKLF 4

REM  a15_13+14.res in Pnma
REM R1 =  0.0283 for    2932 Fo > 4sig(Fo)  and  0.0325 for all    3287 data
REM     67 parameters refined using      0 restraints

END

WGHT      0.0354      0.2389

REM Highest difference peak  0.711,  deepest hole -1.014,  1-sigma level  0.091
Q1    1   0.5021  0.9082  0.2833  11.00000  0.05    0.71
Q2    1   0.2405  0.5870  0.5853  11.00000  0.05    0.63
Q3    1   0.2505  0.7500  0.1095  10.50000  0.05    0.63
Q4    1   0.4381  0.8317  0.3333  11.00000  0.05    0.60
Q5    1   0.2992  0.8372  0.5252  11.00000  0.05    0.58
Q6    1   0.4774  0.7500  0.7792  10.50000  0.05    0.53
Q7    1   0.3699  0.7500  0.6170  10.50000  0.05    0.43
Q8    1   0.3748  0.7500  0.1947  10.50000  0.05    0.42
Q9    1   0.2976  0.7500  0.2635  10.50000  0.05    0.42
Q10   1   0.4394  0.7500  0.2561  10.50000  0.05    0.38
Q11   1   0.4476  0.7722  0.6077  11.00000  0.05    0.36
Q12   1   0.3771  0.7905  0.5227  11.00000  0.05    0.32
Q13   1   0.3616  0.8343  0.4458  11.00000  0.05    0.31
Q14   1   0.3501  0.7829  0.3993  11.00000  0.05    0.31
Q15   1   0.4845  0.7901  0.8453  11.00000  0.05    0.30
Q16   1   0.3486  0.7500  0.0468  10.50000  0.05    0.28
Q17   1   0.5480  0.9851  0.2098  11.00000  0.05    0.28
Q18   1   0.3585  0.7500  0.5074  10.50000  0.05    0.27
Q19   1   0.6542  0.7500  0.7607  10.50000  0.05    0.27
Q20   1   0.3422  0.7500 -0.1518  10.50000  0.05    0.27
;
_shelx_res_checksum              37875
