# 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_5
_database_code_depnum_ccdc_archive 'CCDC 1026104'
_audit_update_record             
;
2014-09-25 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H26 O3'
_chemical_formula_sum            'C19 H26 O3'
_chemical_formula_weight         302.40

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9457(4)
_cell_length_b                   9.2864(5)
_cell_length_c                   11.7075(5)
_cell_angle_alpha                100.602(4)
_cell_angle_beta                 98.957(4)
_cell_angle_gamma                115.369(5)
_cell_volume                     833.13(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7418
_cell_measurement_theta_min      3.9743
_cell_measurement_theta_max      73.5548

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             328
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.49196
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
;
 Oxford Diffraction Xcalibur Nova
;
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.2640
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7829
_diffrn_reflns_av_R_equivalents  0.0112
_diffrn_reflns_av_sigmaI/netI    0.0090
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.98
_diffrn_reflns_theta_max         73.79
_reflns_number_total             3068
_reflns_number_gt                2939
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2006)'
_computing_publication_material  'SHELXL-97(Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0522P)²+0.2986P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3068
_refine_ls_number_parameters     201
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1104
_refine_ls_wR_factor_gt          0.1036
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.87734(12) 0.08035(11) 0.22746(8) 0.0324(2) Uani 1 1 d . . .
O2 O 0.86649(14) 0.62754(12) 0.24224(9) 0.0398(3) Uani 1 1 d . . .
O3 O 0.89357(14) 0.61902(12) 0.43357(9) 0.0408(3) Uani 1 1 d . . .
C1 C 0.79124(16) 0.13444(15) 0.14580(11) 0.0284(3) Uani 1 1 d . . .
H1 H 0.7791 0.0811 0.0621 0.034 Uiso 1 1 calc R . .
C12 C 1.07588(16) 0.39538(14) 0.17727(11) 0.0271(3) Uani 1 1 d . . .
C10 C 0.88765(15) 0.32467(14) 0.17377(11) 0.0267(3) Uani 1 1 d . . .
H10 H 0.8328 0.3561 0.1107 0.032 Uiso 1 1 calc R . .
C2 C 0.61623(16) 0.10018(15) 0.16737(11) 0.0284(3) Uani 1 1 d . . .
H2 H 0.5494 0.1060 0.0953 0.034 Uiso 1 1 calc R . .
C16 C 1.37472(18) 0.50966(18) 0.28190(14) 0.0383(3) Uani 1 1 d . . .
H16 H 1.4589 0.5470 0.3537 0.046 Uiso 1 1 calc R . .
C11 C 0.87011(15) 0.55377(15) 0.31600(11) 0.0271(3) Uani 1 1 d . . .
C3 C 0.51539(18) -0.07380(16) 0.18034(13) 0.0356(3) Uani 1 1 d . . .
H3A H 0.5027 -0.1541 0.1087 0.043 Uiso 1 1 calc R . .
H3B H 0.5821 -0.0857 0.2482 0.043 Uiso 1 1 calc R . .
C8 C 0.65151(16) 0.25111(15) 0.27218(12) 0.0285(3) Uani 1 1 d . . .
H8 H 0.5806 0.3002 0.2436 0.034 Uiso 1 1 calc R . .
C5 C 0.33725(18) -0.06185(18) 0.32866(14) 0.0400(3) Uani 1 1 d . . .
H5B H 0.3916 -0.1105 0.3758 0.048 Uiso 1 1 calc R . .
H5A H 0.2191 -0.1067 0.3331 0.048 Uiso 1 1 calc R . .
C4 C 0.33761(17) -0.11651(17) 0.19879(13) 0.0378(3) Uani 1 1 d . . .
H4A H 0.2874 -0.0648 0.1517 0.045 Uiso 1 1 calc R . .
H4B H 0.2654 -0.2358 0.1681 0.045 Uiso 1 1 calc R . .
C9 C 0.84355(15) 0.37843(14) 0.29011(11) 0.0260(3) Uani 1 1 d . . .
H9 H 0.9151 0.3689 0.3577 0.031 Uiso 1 1 calc R . .
C14 C 1.20441(17) 0.45199(16) 0.28334(12) 0.0336(3) Uani 1 1 d . . .
H14 H 1.1755 0.4511 0.3563 0.040 Uiso 1 1 calc R . .
C13 C 1.12370(17) 0.39899(16) 0.06975(12) 0.0318(3) Uani 1 1 d . . .
H13 H 1.0400 0.3625 -0.0021 0.038 Uiso 1 1 calc R . .
C15 C 1.29379(18) 0.45599(18) 0.06810(13) 0.0373(3) Uani 1 1 d . . .
H15 H 1.3232 0.4566 -0.0046 0.045 Uiso 1 1 calc R . .
C19 C 0.9118(2) 0.78466(18) 0.46733(15) 0.0454(4) Uani 1 1 d . . .
H19A H 1.0079 0.8591 0.4443 0.068 Uiso 1 1 calc R . .
H19B H 0.9303 0.8208 0.5529 0.068 Uiso 1 1 calc R . .
H19C H 0.8094 0.7841 0.4272 0.068 Uiso 1 1 calc R . .
C18 C 0.9589(2) -0.0043(2) 0.17409(16) 0.0520(4) Uani 1 1 d . . .
H18C H 0.8767 -0.0966 0.1072 0.078 Uiso 1 1 calc R . .
H18A H 1.0065 -0.0440 0.2325 0.078 Uiso 1 1 calc R . .
H18B H 1.0491 0.0701 0.1462 0.078 Uiso 1 1 calc R . .
C17 C 1.42033(18) 0.51208(17) 0.17456(14) 0.0378(3) Uani 1 1 d . . .
H17 H 1.5347 0.5509 0.1737 0.045 Uiso 1 1 calc R . .
C7 C 0.61697(18) 0.21605(18) 0.39021(13) 0.0370(3) Uani 1 1 d . . .
H7A H 0.6709 0.3207 0.4528 0.044 Uiso 1 1 calc R . .
H7B H 0.6708 0.1504 0.4122 0.044 Uiso 1 1 calc R . .
C6 C 0.42654(19) 0.12437(19) 0.38663(14) 0.0422(4) Uani 1 1 d . . .
H6B H 0.4160 0.1443 0.4685 0.051 Uiso 1 1 calc R . .
H6A H 0.3667 0.1721 0.3433 0.051 Uiso 1 1 calc R . .


_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
O1 C18 1.4121(17) . ?
O1 C1 1.4277(15) . ?
O2 C11 1.2016(16) . ?
O3 C11 1.3416(16) . ?
O3 C19 1.4456(16) . ?
C1 C2 1.5303(17) . ?
C1 C10 1.5380(16) . ?
C1 H1 0.9800 . ?
C12 C14 1.3920(19) . ?
C12 C13 1.3926(18) . ?
C12 C10 1.5130(17) . ?
C10 C9 1.5316(17) . ?
C10 H10 0.9800 . ?
C2 C3 1.5269(17) . ?
C2 C8 1.5612(17) . ?
C2 H2 0.9800 . ?
C16 C17 1.382(2) . ?
C16 C14 1.3859(19) . ?
C16 H16 0.9300 . ?
C11 C9 1.5047(16) . ?
C3 C4 1.5268(19) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C8 C7 1.5242(18) . ?
C8 C9 1.5650(16) . ?
C8 H8 0.9800 . ?
C5 C4 1.513(2) . ?
C5 C6 1.518(2) . ?
C5 H5B 0.9700 . ?
C5 H5A 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C9 H9 0.9800 . ?
C14 H14 0.9300 . ?
C13 C15 1.3851(19) . ?
C13 H13 0.9300 . ?
C15 C17 1.387(2) . ?
C15 H15 0.9300 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C18 H18C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C17 H17 0.9300 . ?
C7 C6 1.5332(19) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C6 H6B 0.9700 . ?
C6 H6A 0.9700 . ?

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
C18 O1 C1 114.09(11) . . ?
C11 O3 C19 115.93(11) . . ?
O1 C1 C2 110.21(10) . . ?
O1 C1 C10 110.12(10) . . ?
C2 C1 C10 103.36(10) . . ?
O1 C1 H1 111.0 . . ?
C2 C1 H1 111.0 . . ?
C10 C1 H1 111.0 . . ?
C14 C12 C13 117.99(12) . . ?
C14 C12 C10 122.85(11) . . ?
C13 C12 C10 119.12(11) . . ?
C12 C10 C9 117.02(10) . . ?
C12 C10 C1 114.48(10) . . ?
C9 C10 C1 101.41(9) . . ?
C12 C10 H10 107.8 . . ?
C9 C10 H10 107.8 . . ?
C1 C10 H10 107.8 . . ?
C3 C2 C1 113.03(10) . . ?
C3 C2 C8 117.81(11) . . ?
C1 C2 C8 105.70(10) . . ?
C3 C2 H2 106.5 . . ?
C1 C2 H2 106.5 . . ?
C8 C2 H2 106.5 . . ?
C17 C16 C14 120.43(13) . . ?
C17 C16 H16 119.8 . . ?
C14 C16 H16 119.8 . . ?
O2 C11 O3 122.89(11) . . ?
O2 C11 C9 125.61(12) . . ?
O3 C11 C9 111.46(10) . . ?
C4 C3 C2 115.33(11) . . ?
C4 C3 H3A 108.4 . . ?
C2 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
C2 C3 H3B 108.4 . . ?
H3A C3 H3B 107.5 . . ?
C7 C8 C2 116.98(11) . . ?
C7 C8 C9 111.57(10) . . ?
C2 C8 C9 104.35(9) . . ?
C7 C8 H8 107.9 . . ?
C2 C8 H8 107.9 . . ?
C9 C8 H8 107.9 . . ?
C4 C5 C6 115.81(12) . . ?
C4 C5 H5B 108.3 . . ?
C6 C5 H5B 108.3 . . ?
C4 C5 H5A 108.3 . . ?
C6 C5 H5A 108.3 . . ?
H5B C5 H5A 107.4 . . ?
C5 C4 C3 114.15(12) . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4B 108.7 . . ?
C3 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C11 C9 C10 112.68(10) . . ?
C11 C9 C8 111.43(10) . . ?
C10 C9 C8 105.39(10) . . ?
C11 C9 H9 109.1 . . ?
C10 C9 H9 109.1 . . ?
C8 C9 H9 109.1 . . ?
C16 C14 C12 120.99(12) . . ?
C16 C14 H14 119.5 . . ?
C12 C14 H14 119.5 . . ?
C15 C13 C12 121.10(13) . . ?
C15 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C15 C17 120.21(13) . . ?
C13 C15 H15 119.9 . . ?
C17 C15 H15 119.9 . . ?
O3 C19 H19A 109.5 . . ?
O3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
O3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O1 C18 H18C 109.5 . . ?
O1 C18 H18A 109.5 . . ?
H18C C18 H18A 109.5 . . ?
O1 C18 H18B 109.5 . . ?
H18C C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C17 C15 119.29(13) . . ?
C16 C17 H17 120.4 . . ?
C15 C17 H17 120.4 . . ?
C8 C7 C6 114.62(12) . . ?
C8 C7 H7A 108.6 . . ?
C6 C7 H7A 108.6 . . ?
C8 C7 H7B 108.6 . . ?
C6 C7 H7B 108.6 . . ?
H7A C7 H7B 107.6 . . ?
C5 C6 C7 115.53(12) . . ?
C5 C6 H6B 108.4 . . ?
C7 C6 H6B 108.4 . . ?
C5 C6 H6A 108.4 . . ?
C7 C6 H6A 108.4 . . ?
H6B C6 H6A 107.5 . . ?

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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C18 O1 C1 C2 137.03(12) . . . . ?
C18 O1 C1 C10 -109.57(13) . . . . ?
C14 C12 C10 C9 24.22(17) . . . . ?
C13 C12 C10 C9 -158.22(11) . . . . ?
C14 C12 C10 C1 -94.22(14) . . . . ?
C13 C12 C10 C1 83.33(14) . . . . ?
O1 C1 C10 C12 53.71(14) . . . . ?
C2 C1 C10 C12 171.43(10) . . . . ?
O1 C1 C10 C9 -73.25(12) . . . . ?
C2 C1 C10 C9 44.47(12) . . . . ?
O1 C1 C2 C3 -45.91(14) . . . . ?
C10 C1 C2 C3 -163.57(11) . . . . ?
O1 C1 C2 C8 84.34(11) . . . . ?
C10 C1 C2 C8 -33.32(12) . . . . ?
C19 O3 C11 O2 0.99(19) . . . . ?
C19 O3 C11 C9 -177.04(11) . . . . ?
C1 C2 C3 C4 -178.48(11) . . . . ?
C8 C2 C3 C4 57.69(16) . . . . ?
C3 C2 C8 C7 12.79(17) . . . . ?
C1 C2 C8 C7 -114.64(12) . . . . ?
C3 C2 C8 C9 136.58(11) . . . . ?
C1 C2 C8 C9 9.15(12) . . . . ?
C6 C5 C4 C3 65.61(17) . . . . ?
C2 C3 C4 C5 -85.63(15) . . . . ?
O2 C11 C9 C10 25.07(17) . . . . ?
O3 C11 C9 C10 -156.97(10) . . . . ?
O2 C11 C9 C8 -93.16(15) . . . . ?
O3 C11 C9 C8 84.79(13) . . . . ?
C12 C10 C9 C11 74.21(13) . . . . ?
C1 C10 C9 C11 -160.51(10) . . . . ?
C12 C10 C9 C8 -164.07(10) . . . . ?
C1 C10 C9 C8 -38.79(12) . . . . ?
C7 C8 C9 C11 -91.74(13) . . . . ?
C2 C8 C9 C11 141.05(10) . . . . ?
C7 C8 C9 C10 145.73(11) . . . . ?
C2 C8 C9 C10 18.51(12) . . . . ?
C17 C16 C14 C12 0.0(2) . . . . ?
C13 C12 C14 C16 -0.22(19) . . . . ?
C10 C12 C14 C16 177.36(12) . . . . ?
C14 C12 C13 C15 0.47(19) . . . . ?
C10 C12 C13 C15 -177.21(11) . . . . ?
C12 C13 C15 C17 -0.5(2) . . . . ?
C14 C16 C17 C15 -0.1(2) . . . . ?
C13 C15 C17 C16 0.3(2) . . . . ?
C2 C8 C7 C6 -73.02(16) . . . . ?
C9 C8 C7 C6 166.95(11) . . . . ?
C4 C5 C6 C7 -59.39(18) . . . . ?
C8 C7 C6 C5 79.51(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.912
_diffrn_reflns_theta_full        70.00
_diffrn_measured_fraction_theta_full 0.945
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.037
#===END
####################################################################### 
# 
# 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_3d
_database_code_depnum_ccdc_archive 'CCDC 1026105'
_audit_update_record             
;
2014-09-25 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H18 Cr O8'
_chemical_formula_sum            'C22 H18 Cr O8'
_chemical_formula_weight         462.36

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'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   12.5048(2)
_cell_length_b                   16.5248(3)
_cell_length_c                   21.1589(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4372.26(13)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4569
_cell_measurement_theta_min      1.018
_cell_measurement_theta_max      25.082

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1904
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.912
_exptl_absorpt_correction_T_max  1.047
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_device       '95 mm CCD camera on κ-goniostat'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21876
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.92
_diffrn_reflns_theta_max         25.24
_reflns_number_total             3946
_reflns_number_gt                3061
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2002)'
_computing_cell_refinement       'HKL SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        
'HKL DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1135P)²+1.5047P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3946
_refine_ls_number_parameters     280
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_ref         0.1776
_refine_ls_wR_factor_gt          0.1449
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.30630(3) 0.14562(3) 0.54180(2) 0.0282(2) Uani 1 1 d . . .
O1 O 0.29578(16) 0.23537(12) 0.41527(10) 0.0388(5) Uani 1 1 d . . .
O2 O 0.37584(15) -0.02904(12) 0.31918(9) 0.0359(5) Uani 1 1 d . . .
O5 O 0.22808(16) -0.02549(13) 0.51560(10) 0.0402(5) Uani 1 1 d . . .
O3 O 0.11239(14) 0.08060(13) 0.40748(10) 0.0374(5) Uani 1 1 d . . .
O6 O 0.07439(17) 0.20303(14) 0.54034(11) 0.0463(6) Uani 1 1 d . . .
O4 O 0.53563(16) 0.08318(14) 0.53897(10) 0.0429(6) Uani 1 1 d . . .
O8 O 0.3994(2) 0.30412(16) 0.58975(14) 0.0653(8) Uani 1 1 d . . .
O7 O 0.2865(2) 0.10100(19) 0.68042(11) 0.0611(7) Uani 1 1 d . . .
C12 C 0.1805(2) 0.04092(19) 0.36602(13) 0.0321(6) Uani 1 1 d . . .
C6 C 0.2758(2) 0.08824(17) 0.34707(13) 0.0297(6) Uani 1 1 d . . .
H6 H 0.2500 0.1398 0.3301 0.036 Uiso 1 1 calc R . .
C5 C 0.3452(2) 0.04929(18) 0.29611(13) 0.0330(6) Uani 1 1 d . . .
H5 H 0.3083 0.0461 0.2553 0.040 Uiso 1 1 calc R . .
C4 C 0.4380(2) 0.10668(17) 0.29438(13) 0.0321(6) Uani 1 1 d . . .
C3 C 0.4573(2) 0.13879(17) 0.36023(13) 0.0303(6) Uani 1 1 d . . .
H3 H 0.4575 0.1981 0.3593 0.036 Uiso 1 1 calc R . .
C13 C 0.1390(2) -0.0314(2) 0.35037(15) 0.0401(7) Uani 1 1 d . . .
H13 H 0.1689 -0.0693 0.3232 0.048 Uiso 1 1 calc R . .
C10 C 0.5857(3) 0.1859(2) 0.24915(17) 0.0479(8) Uani 1 1 d . . .
H10 H 0.5970 0.2222 0.2162 0.057 Uiso 1 1 calc R . .
C19 C 0.2944(2) 0.1178(2) 0.62819(16) 0.0406(7) Uani 1 1 d . . .
C8 C 0.6548(3) 0.1357(2) 0.35199(16) 0.0434(8) Uani 1 1 d . . .
H8 H 0.7201 0.1198 0.3691 0.052 Uiso 1 1 calc R . .
C9 C 0.6567(3) 0.1872(2) 0.29706(17) 0.0482(8) Uani 1 1 d . . .
H9 H 0.7118 0.2248 0.2944 0.058 Uiso 1 1 calc R . .
C11 C 0.4934(2) 0.13316(19) 0.24404(14) 0.0398(7) Uani 1 1 d . . .
H11 H 0.4715 0.1169 0.2040 0.048 Uiso 1 1 calc R . .
C15 C 0.0278(2) 0.0292(2) 0.41713(15) 0.0459(8) Uani 1 1 d . . .
H15 H -0.0300 0.0403 0.4434 0.055 Uiso 1 1 calc R . .
C1 C 0.3193(2) 0.17023(18) 0.44752(14) 0.0306(6) Uani 1 1 d . . .
C22 C 0.4434(2) -0.0722(2) 0.27661(17) 0.0484(8) Uani 1 1 d . . .
H22B H 0.4611 -0.1239 0.2945 0.073 Uiso 1 1 calc R . .
H22A H 0.5077 -0.0419 0.2695 0.073 Uiso 1 1 calc R . .
H22C H 0.4068 -0.0800 0.2372 0.073 Uiso 1 1 calc R . .
C2 C 0.3597(2) 0.10859(17) 0.39972(12) 0.0271(6) Uani 1 1 d . . .
H2 H 0.3794 0.0587 0.4219 0.033 Uiso 1 1 calc R . .
C14 C 0.0396(2) -0.0387(2) 0.38373(16) 0.0463(8) Uani 1 1 d . . .
H14 H -0.0074 -0.0823 0.3824 0.056 Uiso 1 1 calc R . .
C7 C 0.5650(2) 0.10899(19) 0.38030(14) 0.0356(7) Uani 1 1 d . . .
H7 H 0.5701 0.0714 0.4129 0.043 Uiso 1 1 calc R . .
C18 C 0.1620(3) 0.18338(18) 0.54090(13) 0.0325(6) Uani 1 1 d . . .
C21 C 0.2594(4) 0.3095(2) 0.44432(18) 0.0604(11) Uani 1 1 d . . .
H21B H 0.2463 0.3493 0.4122 0.091 Uiso 1 1 calc R . .
H21A H 0.3132 0.3291 0.4729 0.091 Uiso 1 1 calc R . .
H21C H 0.1945 0.2993 0.4672 0.091 Uiso 1 1 calc R . .
C20 C 0.3620(2) 0.2469(2) 0.56899(16) 0.0432(8) Uani 1 1 d . . .
C17 C 0.2564(2) 0.03932(18) 0.52312(13) 0.0312(6) Uani 1 1 d . . .
C16 C 0.4494(2) 0.10668(19) 0.53982(12) 0.0328(7) Uani 1 1 d . . .


_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 C19 1.891(3) . ?
Cr1 C20 1.902(3) . ?
Cr1 C16 1.902(3) . ?
Cr1 C17 1.906(3) . ?
Cr1 C18 1.909(3) . ?
Cr1 C1 2.042(3) . ?
O1 C1 1.308(4) . ?
O1 C21 1.444(4) . ?
O2 C22 1.427(3) . ?
O2 C5 1.435(3) . ?
O5 C17 1.139(3) . ?
O3 C15 1.372(4) . ?
O3 C12 1.387(3) . ?
O6 C18 1.143(4) . ?
O4 C16 1.147(4) . ?
O8 C20 1.143(4) . ?
O7 C19 1.144(4) . ?
C12 C13 1.344(4) . ?
C12 C6 1.481(4) . ?
C6 C5 1.527(4) . ?
C6 C2 1.567(4) . ?
C6 H6 0.9800 . ?
C5 C4 1.499(4) . ?
C5 H5 0.9800 . ?
C4 C11 1.344(4) . ?
C4 C3 1.510(4) . ?
C3 C7 1.496(4) . ?
C3 C2 1.561(4) . ?
C3 H3 0.9800 . ?
C13 C14 1.434(4) . ?
C13 H13 0.9300 . ?
C10 C9 1.347(5) . ?
C10 C11 1.449(5) . ?
C10 H10 0.9300 . ?
C8 C7 1.347(4) . ?
C8 C9 1.441(5) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C11 H11 0.9300 . ?
C15 C14 1.335(5) . ?
C15 H15 0.9300 . ?
C1 C2 1.522(4) . ?
C22 H22B 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22C 0.9600 . ?
C2 H2 0.9800 . ?
C14 H14 0.9300 . ?
C7 H7 0.9300 . ?
C21 H21B 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21C 0.9600 . ?

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
C19 Cr1 C20 87.17(15) . . ?
C19 Cr1 C16 90.74(12) . . ?
C20 Cr1 C16 87.68(13) . . ?
C19 Cr1 C17 87.16(14) . . ?
C20 Cr1 C17 173.64(14) . . ?
C16 Cr1 C17 89.51(12) . . ?
C19 Cr1 C18 90.86(12) . . ?
C20 Cr1 C18 93.54(13) . . ?
C16 Cr1 C18 178.03(12) . . ?
C17 Cr1 C18 89.42(12) . . ?
C19 Cr1 C1 177.39(14) . . ?
C20 Cr1 C1 95.23(14) . . ?
C16 Cr1 C1 88.34(11) . . ?
C17 Cr1 C1 90.40(12) . . ?
C18 Cr1 C1 90.02(11) . . ?
C1 O1 C21 123.1(2) . . ?
C22 O2 C5 113.2(2) . . ?
C15 O3 C12 106.0(2) . . ?
C13 C12 O3 109.8(2) . . ?
C13 C12 C6 135.5(3) . . ?
O3 C12 C6 114.6(3) . . ?
C12 C6 C5 115.2(2) . . ?
C12 C6 C2 117.4(2) . . ?
C5 C6 C2 102.2(2) . . ?
C12 C6 H6 107.1 . . ?
C5 C6 H6 107.1 . . ?
C2 C6 H6 107.1 . . ?
O2 C5 C4 111.9(2) . . ?
O2 C5 C6 107.0(2) . . ?
C4 C5 C6 101.0(2) . . ?
O2 C5 H5 112.1 . . ?
C4 C5 H5 112.1 . . ?
C6 C5 H5 112.1 . . ?
C11 C4 C5 128.7(3) . . ?
C11 C4 C3 122.3(3) . . ?
C5 C4 C3 108.9(2) . . ?
C7 C3 C4 106.9(2) . . ?
C7 C3 C2 116.5(2) . . ?
C4 C3 C2 104.9(2) . . ?
C7 C3 H3 109.4 . . ?
C4 C3 H3 109.4 . . ?
C2 C3 H3 109.4 . . ?
C12 C13 C14 106.8(3) . . ?
C12 C13 H13 126.6 . . ?
C14 C13 H13 126.6 . . ?
C9 C10 C11 126.2(3) . . ?
C9 C10 H10 116.9 . . ?
C11 C10 H10 116.9 . . ?
O7 C19 Cr1 179.5(3) . . ?
C7 C8 C9 124.4(3) . . ?
C7 C8 H8 117.8 . . ?
C9 C8 H8 117.8 . . ?
C10 C9 C8 125.9(3) . . ?
C10 C9 H9 117.0 . . ?
C8 C9 H9 117.0 . . ?
C4 C11 C10 123.2(3) . . ?
C4 C11 H11 118.4 . . ?
C10 C11 H11 118.4 . . ?
C14 C15 O3 110.9(3) . . ?
C14 C15 H15 124.6 . . ?
O3 C15 H15 124.6 . . ?
O1 C1 C2 106.2(2) . . ?
O1 C1 Cr1 131.0(2) . . ?
C2 C1 Cr1 122.8(2) . . ?
O2 C22 H22B 109.5 . . ?
O2 C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
O2 C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
C1 C2 C3 113.7(2) . . ?
C1 C2 C6 113.2(2) . . ?
C3 C2 C6 102.2(2) . . ?
C1 C2 H2 109.2 . . ?
C3 C2 H2 109.2 . . ?
C6 C2 H2 109.2 . . ?
C15 C14 C13 106.6(3) . . ?
C15 C14 H14 126.7 . . ?
C13 C14 H14 126.7 . . ?
C8 C7 C3 121.1(3) . . ?
C8 C7 H7 119.4 . . ?
C3 C7 H7 119.4 . . ?
O6 C18 Cr1 177.4(3) . . ?
O1 C21 H21B 109.5 . . ?
O1 C21 H21A 109.5 . . ?
H21B C21 H21A 109.5 . . ?
O1 C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
O8 C20 Cr1 173.9(3) . . ?
O5 C17 Cr1 175.9(3) . . ?
O4 C16 Cr1 179.6(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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C15 O3 C12 C13 0.6(3) . . . . ?
C15 O3 C12 C6 177.4(2) . . . . ?
C13 C12 C6 C5 2.1(5) . . . . ?
O3 C12 C6 C5 -173.7(2) . . . . ?
C13 C12 C6 C2 -118.4(3) . . . . ?
O3 C12 C6 C2 65.8(3) . . . . ?
C22 O2 C5 C4 -69.1(3) . . . . ?
C22 O2 C5 C6 -178.8(2) . . . . ?
C12 C6 C5 O2 -56.5(3) . . . . ?
C2 C6 C5 O2 72.0(2) . . . . ?
C12 C6 C5 C4 -173.6(2) . . . . ?
C2 C6 C5 C4 -45.1(3) . . . . ?
O2 C5 C4 C11 105.4(3) . . . . ?
C6 C5 C4 C11 -141.1(3) . . . . ?
O2 C5 C4 C3 -79.5(3) . . . . ?
C6 C5 C4 C3 34.0(3) . . . . ?
C11 C4 C3 C7 -69.2(3) . . . . ?
C5 C4 C3 C7 115.4(3) . . . . ?
C11 C4 C3 C2 166.5(3) . . . . ?
C5 C4 C3 C2 -8.9(3) . . . . ?
O3 C12 C13 C14 -0.4(3) . . . . ?
C6 C12 C13 C14 -176.3(3) . . . . ?
C20 Cr1 C19 O7 104(40) . . . . ?
C16 Cr1 C19 O7 -168(100) . . . . ?
C17 Cr1 C19 O7 -79(40) . . . . ?
C18 Cr1 C19 O7 10(40) . . . . ?
C1 Cr1 C19 O7 -99(40) . . . . ?
C11 C10 C9 C8 0.8(5) . . . . ?
C7 C8 C9 C10 -34.4(5) . . . . ?
C5 C4 C11 C10 -176.7(3) . . . . ?
C3 C4 C11 C10 8.8(4) . . . . ?
C9 C10 C11 C4 31.8(5) . . . . ?
C12 O3 C15 C14 -0.6(3) . . . . ?
C21 O1 C1 C2 -176.9(3) . . . . ?
C21 O1 C1 Cr1 4.3(4) . . . . ?
C19 Cr1 C1 O1 159(2) . . . . ?
C20 Cr1 C1 O1 -43.7(3) . . . . ?
C16 Cr1 C1 O1 -131.2(3) . . . . ?
C17 Cr1 C1 O1 139.3(3) . . . . ?
C18 Cr1 C1 O1 49.9(3) . . . . ?
C19 Cr1 C1 C2 -19(3) . . . . ?
C20 Cr1 C1 C2 137.7(2) . . . . ?
C16 Cr1 C1 C2 50.2(2) . . . . ?
C17 Cr1 C1 C2 -39.3(2) . . . . ?
C18 Cr1 C1 C2 -128.7(2) . . . . ?
O1 C1 C2 C3 57.0(3) . . . . ?
Cr1 C1 C2 C3 -124.1(2) . . . . ?
O1 C1 C2 C6 -59.0(3) . . . . ?
Cr1 C1 C2 C6 119.9(2) . . . . ?
C7 C3 C2 C1 100.6(3) . . . . ?
C4 C3 C2 C1 -141.4(2) . . . . ?
C7 C3 C2 C6 -137.0(2) . . . . ?
C4 C3 C2 C6 -19.1(3) . . . . ?
C12 C6 C2 C1 -70.3(3) . . . . ?
C5 C6 C2 C1 162.6(2) . . . . ?
C12 C6 C2 C3 167.0(2) . . . . ?
C5 C6 C2 C3 39.9(3) . . . . ?
O3 C15 C14 C13 0.4(3) . . . . ?
C12 C13 C14 C15 0.0(3) . . . . ?
C9 C8 C7 C3 -6.7(5) . . . . ?
C4 C3 C7 C8 67.6(3) . . . . ?
C2 C3 C7 C8 -175.6(3) . . . . ?
C19 Cr1 C18 O6 -76(5) . . . . ?
C20 Cr1 C18 O6 -163(5) . . . . ?
C16 Cr1 C18 O6 69(7) . . . . ?
C17 Cr1 C18 O6 12(5) . . . . ?
C1 Cr1 C18 O6 102(5) . . . . ?
C19 Cr1 C20 O8 33(3) . . . . ?
C16 Cr1 C20 O8 -58(3) . . . . ?
C17 Cr1 C20 O8 6(3) . . . . ?
C18 Cr1 C20 O8 124(3) . . . . ?
C1 Cr1 C20 O8 -146(3) . . . . ?
C19 Cr1 C17 O5 -17(3) . . . . ?
C20 Cr1 C17 O5 10(4) . . . . ?
C16 Cr1 C17 O5 74(3) . . . . ?
C18 Cr1 C17 O5 -108(3) . . . . ?
C1 Cr1 C17 O5 162(3) . . . . ?
C19 Cr1 C16 O4 -12(88) . . . . ?
C20 Cr1 C16 O4 75(100) . . . . ?
C17 Cr1 C16 O4 -100(88) . . . . ?
C18 Cr1 C16 O4 -157(100) . . . . ?
C1 Cr1 C16 O4 170(100) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.255
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.167
#===END
