# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_1-153k
_database_code_depnum_ccdc_archive 'CCDC 1531724'
_audit_update_record             
;
2017-02-08 deposited with the CCDC.	2021-06-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H64 Br2 Cr2 N2 O18'
_chemical_formula_weight         980.63

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'
N N 0.0311 0.0180 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -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, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   16.6558(3)
_cell_length_b                   11.3245(3)
_cell_length_c                   23.4109(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4415.73(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12551
_cell_measurement_theta_min      3.8060
_cell_measurement_theta_max      77.2090

_exptl_crystal_description       column
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             2032
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    6.756
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26717
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_av_R_equivalents  0.0913
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.776
_diffrn_reflns_theta_max         62.991
_diffrn_reflns_theta_full        62.991
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             6757
_reflns_number_gt                5230
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.947
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_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 FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1840P)²+1.9500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.46(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6757
_refine_ls_number_parameters     499
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0799
_refine_ls_wR_factor_ref         0.2632
_refine_ls_wR_factor_gt          0.2401
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.039
_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_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
Br1 Br 0.42566(13) 0.74767(18) 0.82436(7) 0.0851(7) Uani 1 1 d . . . . .
N1 N 0.5425(6) 0.7608(8) 0.5169(4) 0.046(2) Uani 1 1 d . . . . .
H1C H 0.5812 0.8150 0.5179 0.069 Uiso 1 1 calc R U . . .
H1D H 0.5620 0.6919 0.5290 0.069 Uiso 1 1 calc R U . . .
H1E H 0.5245 0.7531 0.4813 0.069 Uiso 1 1 calc R U . . .
N2 N 0.2059(6) 0.2675(8) 0.7549(5) 0.048(2) Uani 1 1 d . . . . .
H2C H 0.1653 0.3172 0.7491 0.072 Uiso 1 1 calc R U . . .
H2D H 0.1887 0.1936 0.7506 0.072 Uiso 1 1 calc R U . . .
H2E H 0.2248 0.2771 0.7901 0.072 Uiso 1 1 calc R U . . .
C1 C 0.5488(8) 1.0742(10) 0.4770(5) 0.053(3) Uani 1 1 d . . . . .
H1A H 0.5060 1.0717 0.5051 0.064 Uiso 1 1 calc R U . . .
H1B H 0.5427 1.1456 0.4545 0.064 Uiso 1 1 calc R U . . .
C2 C 0.6290(7) 1.0740(10) 0.5064(5) 0.051(3) Uani 1 1 d . . . . .
H2A H 0.6717 1.0698 0.4783 0.061 Uiso 1 1 calc R U . . .
H2B H 0.6357 1.1459 0.5283 0.061 Uiso 1 1 calc R U . . .
C3 C 0.7093(8) 0.9645(11) 0.5723(6) 0.061(3) Uani 1 1 d . . . . .
H3A H 0.7195 1.0352 0.5945 0.073 Uiso 1 1 calc R U . . .
H3B H 0.7521 0.9553 0.5446 0.073 Uiso 1 1 calc R U . . .
C4 C 0.7058(7) 0.8619(11) 0.6096(5) 0.057(3) Uani 1 1 d . . . . .
H4A H 0.7542 0.8586 0.6327 0.068 Uiso 1 1 calc R U . . .
H4B H 0.6603 0.8692 0.6352 0.068 Uiso 1 1 calc R U . . .
C5 C 0.6958(7) 0.6525(12) 0.6121(5) 0.058(3) Uani 1 1 d . . . . .
H5A H 0.6484 0.6551 0.6361 0.070 Uiso 1 1 calc R U . . .
H5B H 0.7427 0.6506 0.6367 0.070 Uiso 1 1 calc R U . . .
C6 C 0.6939(9) 0.5467(11) 0.5771(6) 0.063(3) Uani 1 1 d . . . . .
H6A H 0.6998 0.4773 0.6011 0.076 Uiso 1 1 calc R U . . .
H6B H 0.7380 0.5479 0.5500 0.076 Uiso 1 1 calc R U . . .
C7 C 0.6118(8) 0.4393(10) 0.5106(5) 0.054(3) Uani 1 1 d . . . . .
H7A H 0.6135 0.3681 0.5336 0.064 Uiso 1 1 calc R U . . .
H7B H 0.6565 0.4375 0.4840 0.064 Uiso 1 1 calc R U . . .
C8 C 0.5351(9) 0.4452(10) 0.4788(5) 0.056(3) Uani 1 1 d . . . . .
H8A H 0.5277 0.3736 0.4566 0.067 Uiso 1 1 calc R U . . .
H8B H 0.4907 0.4522 0.5053 0.067 Uiso 1 1 calc R U . . .
C9 C 0.4713(8) 0.5493(10) 0.4048(5) 0.055(3) Uani 1 1 d . . . . .
H9A H 0.4220 0.5542 0.4267 0.066 Uiso 1 1 calc R U . . .
H9B H 0.4695 0.4778 0.3820 0.066 Uiso 1 1 calc R U . . .
C10 C 0.4784(9) 0.6551(11) 0.3662(6) 0.062(3) Uani 1 1 d . . . . .
H10A H 0.5294 0.6540 0.3462 0.074 Uiso 1 1 calc R U . . .
H10B H 0.4355 0.6552 0.3382 0.074 Uiso 1 1 calc R U . . .
C11 C 0.4751(8) 0.8656(11) 0.3686(6) 0.060(3) Uani 1 1 d . . . . .
H11A H 0.4292 0.8678 0.3432 0.072 Uiso 1 1 calc R U . . .
H11B H 0.5235 0.8670 0.3456 0.072 Uiso 1 1 calc R U . . .
C12 C 0.4735(7) 0.9711(10) 0.4075(6) 0.054(3) Uani 1 1 d . . . . .
H12A H 0.4699 1.0429 0.3851 0.065 Uiso 1 1 calc R U . . .
H12B H 0.4270 0.9671 0.4323 0.065 Uiso 1 1 calc R U . . .
C13 C 0.1254(7) 0.5829(9) 0.7650(5) 0.051(3) Uani 1 1 d . . . . .
H13A H 0.0816 0.5821 0.7924 0.061 Uiso 1 1 calc R U . . .
H13B H 0.1216 0.6552 0.7429 0.061 Uiso 1 1 calc R U . . .
C14 C 0.2049(8) 0.5793(9) 0.7963(5) 0.053(3) Uani 1 1 d . . . . .
H14A H 0.2488 0.5766 0.7690 0.064 Uiso 1 1 calc R U . . .
H14B H 0.2111 0.6495 0.8196 0.064 Uiso 1 1 calc R U . . .
C15 C 0.2775(9) 0.4735(12) 0.8664(7) 0.068(4) Uani 1 1 d . . . . .
H15A H 0.2810 0.5438 0.8899 0.082 Uiso 1 1 calc R U . . .
H15B H 0.3252 0.4690 0.8427 0.082 Uiso 1 1 calc R U . . .
C16 C 0.2701(8) 0.3638(10) 0.9035(5) 0.056(3) Uani 1 1 d . . . . .
H16A H 0.3114 0.3640 0.9327 0.067 Uiso 1 1 calc R U . . .
H16B H 0.2181 0.3625 0.9222 0.067 Uiso 1 1 calc R U . . .
C17 C 0.2730(9) 0.1554(9) 0.9016(5) 0.054(3) Uani 1 1 d . . . . .
H17A H 0.2216 0.1521 0.9210 0.065 Uiso 1 1 calc R U . . .
H17B H 0.3151 0.1537 0.9303 0.065 Uiso 1 1 calc R U . . .
C18 C 0.2815(9) 0.0523(11) 0.8624(7) 0.065(4) Uani 1 1 d . . . . .
H18A H 0.3294 0.0607 0.8392 0.078 Uiso 1 1 calc R U . . .
H18B H 0.2857 -0.0203 0.8842 0.078 Uiso 1 1 calc R U . . .
C19 C 0.2101(10) -0.0519(10) 0.7911(5) 0.060(3) Uani 1 1 d . . . . .
H19A H 0.2152 -0.1232 0.8138 0.072 Uiso 1 1 calc R U . . .
H19B H 0.2543 -0.0492 0.7641 0.072 Uiso 1 1 calc R U . . .
C20 C 0.1337(8) -0.0525(10) 0.7605(5) 0.055(3) Uani 1 1 d . . . . .
H20A H 0.1296 -0.1239 0.7377 0.066 Uiso 1 1 calc R U . . .
H20B H 0.0898 -0.0521 0.7877 0.066 Uiso 1 1 calc R U . . .
C21 C 0.0536(8) 0.0550(11) 0.6972(6) 0.054(3) Uani 1 1 d . . . . .
H21A H 0.0115 0.0606 0.7256 0.065 Uiso 1 1 calc R U . . .
H21B H 0.0449 -0.0161 0.6749 0.065 Uiso 1 1 calc R U . . .
C22 C 0.0516(9) 0.1656(11) 0.6574(6) 0.063(3) Uani 1 1 d . . . . .
H22A H 0.0994 0.1685 0.6338 0.076 Uiso 1 1 calc R U . . .
H22B H 0.0049 0.1632 0.6328 0.076 Uiso 1 1 calc R U . . .
C23 C 0.0411(9) 0.3737(12) 0.6603(6) 0.064(3) Uani 1 1 d . . . . .
H23A H -0.0087 0.3736 0.6388 0.076 Uiso 1 1 calc R U . . .
H23B H 0.0856 0.3801 0.6337 0.076 Uiso 1 1 calc R U . . .
C24 C 0.0424(8) 0.4764(10) 0.7031(5) 0.052(3) Uani 1 1 d . . . . .
H24A H 0.0298 0.5497 0.6836 0.062 Uiso 1 1 calc R U . . .
H24B H 0.0022 0.4634 0.7324 0.062 Uiso 1 1 calc R U . . .
C25 C 0.4727(12) 0.7995(13) 0.5564(7) 0.088(5) Uani 1 1 d . . . . .
H25A H 0.4935 0.7867 0.5946 0.106 Uiso 1 1 d R U . . .
H25B H 0.4585 0.8823 0.5534 0.106 Uiso 1 1 d R U . . .
C26 C 0.4158(14) 0.708(2) 0.5515(12) 0.136(10) Uani 1 1 d . . . . .
H26A H 0.3700 0.7250 0.5750 0.205 Uiso 1 1 calc R U . . .
H26B H 0.3991 0.7006 0.5124 0.205 Uiso 1 1 calc R U . . .
H26C H 0.4396 0.6346 0.5637 0.205 Uiso 1 1 calc R U . . .
C27 C 0.2711(8) 0.2922(16) 0.7125(6) 0.076(4) Uani 1 1 d . . . . .
H27A H 0.2487 0.2842 0.6745 0.092 Uiso 1 1 calc R U . . .
H27B H 0.2875 0.3739 0.7170 0.092 Uiso 1 1 calc R U . . .
C28 C 0.3413(9) 0.2201(19) 0.7158(10) 0.103(7) Uani 1 1 d . . . . .
H28A H 0.3787 0.2438 0.6868 0.155 Uiso 1 1 calc R U . . .
H28B H 0.3656 0.2289 0.7527 0.155 Uiso 1 1 calc R U . . .
H28C H 0.3267 0.1389 0.7100 0.155 Uiso 1 1 calc R U . . .
O1 O 0.6323(5) 0.9741(6) 0.5432(3) 0.0460(17) Uani 1 1 d . . . . .
O2 O 0.6985(5) 0.7550(6) 0.5772(3) 0.0400(16) Uani 1 1 d . . . . .
O3 O 0.6175(5) 0.5419(6) 0.5467(3) 0.0496(18) Uani 1 1 d . . . . .
O4 O 0.5371(5) 0.5451(7) 0.4418(4) 0.0499(18) Uani 1 1 d . . . . .
O5 O 0.4729(6) 0.7588(6) 0.4025(4) 0.0440(19) Uani 1 1 d . . . . .
O6 O 0.5447(5) 0.9725(6) 0.4408(4) 0.0468(17) Uani 1 1 d . . . . .
O7 O 0.2063(5) 0.4770(6) 0.8313(4) 0.0501(19) Uani 1 1 d . . . . .
O8 O 0.2787(6) 0.2637(7) 0.8682(4) 0.050(2) Uani 1 1 d . . . . .
O9 O 0.2121(5) 0.0501(6) 0.8274(4) 0.0485(18) Uani 1 1 d . . . . .
O10 O 0.1278(5) 0.0503(7) 0.7235(4) 0.058(2) Uani 1 1 d . . . . .
O11 O 0.0482(6) 0.2664(7) 0.6944(4) 0.053(2) Uani 1 1 d . . . . .
O12 O 0.1192(5) 0.4846(6) 0.7285(4) 0.0513(19) Uani 1 1 d . . . . .
O25 O 0.4964(6) 0.7325(7) 0.6980(5) 0.063(2) Uani 1 1 d . . . . .
Cr1 Cr 0.41181(16) 0.7170(3) 0.72681(18) 0.0843(10) Uani 1 1 d . . . . .
O26 O 0.3766(8) 0.5838(13) 0.7179(9) 0.160(9) Uani 1 1 d . . . . .
O27 O 0.3512(9) 0.811(2) 0.7042(7) 0.164(8) Uani 1 1 d . . . . .
Br2 Br 0.32528(12) 0.26454(19) 0.44434(7) 0.0880(7) Uani 1 1 d . . . . .
O28 O 0.2533(7) 0.2339(9) 0.5717(6) 0.077(3) Uani 1 1 d . . . . .
Cr2 Cr 0.3404(4) 0.2027(7) 0.5339(7) 0.063(2) Uani 0.62(3) 1 d . . P A 1
O29 O 0.3535(15) 0.0578(15) 0.5248(17) 0.137(14) Uani 0.62(3) 1 d . U P A 1
O30 O 0.4156(16) 0.271(3) 0.5578(12) 0.137(15) Uani 0.62(3) 1 d . U P A 1
Cr2' Cr 0.3368(4) 0.2448(16) 0.5483(2) 0.035(3) Uani 0.38(3) 1 d . . P A 2
O29' O 0.3795(15) 0.117(3) 0.5603(8) 0.065(9) Uani 0.38(3) 1 d . U P A 2
O30' O 0.3886(15) 0.349(3) 0.5716(12) 0.074(10) Uani 0.38(3) 1 d . U P A 2


_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
Br1 Cr1 2.321(5) . ?
N1 C25 1.55(2) . ?
N2 C27 1.498(16) . ?
C1 O6 1.432(14) . ?
C1 C2 1.502(17) . ?
C2 O1 1.423(14) . ?
C3 O1 1.456(16) . ?
C3 C4 1.456(19) . ?
C4 O2 1.434(13) . ?
C5 O2 1.421(13) . ?
C5 C6 1.45(2) . ?
C6 O3 1.460(15) . ?
C7 O3 1.440(15) . ?
C7 C8 1.479(18) . ?
C8 O4 1.425(14) . ?
C9 O4 1.398(14) . ?
C9 C10 1.505(19) . ?
C10 O5 1.453(14) . ?
C11 O5 1.447(14) . ?
C11 C12 1.502(19) . ?
C12 O6 1.418(13) . ?
C13 O12 1.407(15) . ?
C13 C14 1.514(17) . ?
C14 O7 1.419(13) . ?
C15 O7 1.443(16) . ?
C15 C16 1.522(18) . ?
C16 O8 1.410(15) . ?
C17 O8 1.459(14) . ?
C17 C18 1.491(18) . ?
C18 O9 1.418(16) . ?
C19 O9 1.435(13) . ?
C19 C20 1.459(19) . ?
C20 O10 1.454(14) . ?
C21 O10 1.381(15) . ?
C21 C22 1.560(18) . ?
C22 O11 1.434(16) . ?
C23 O11 1.460(14) . ?
C23 C24 1.535(18) . ?
C24 O12 1.414(15) . ?
C25 C26 1.41(3) . ?
C27 C28 1.43(2) . ?
O25 Cr1 1.572(11) . ?
Cr1 O27 1.563(13) . ?
Cr1 O26 1.632(13) . ?
Br2 Cr2 2.224(14) . ?
Br2 Cr2' 2.451(6) . ?
O28 Cr2' 1.499(15) . ?
O28 Cr2 1.735(18) . ?
Cr2 O30 1.572(19) . ?
Cr2 O29 1.670(17) . ?
Cr2' O30' 1.56(2) . ?
Cr2' O29' 1.64(2) . ?

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
O6 C1 C2 108.2(9) . . ?
O1 C2 C1 108.2(10) . . ?
O1 C3 C4 107.8(10) . . ?
O2 C4 C3 111.0(10) . . ?
O2 C5 C6 110.6(10) . . ?
C5 C6 O3 109.0(11) . . ?
O3 C7 C8 108.5(10) . . ?
O4 C8 C7 108.8(9) . . ?
O4 C9 C10 109.7(10) . . ?
O5 C10 C9 106.7(10) . . ?
O5 C11 C12 109.4(10) . . ?
O6 C12 C11 109.1(10) . . ?
O12 C13 C14 109.6(9) . . ?
O7 C14 C13 108.4(9) . . ?
O7 C15 C16 106.3(10) . . ?
O8 C16 C15 108.2(10) . . ?
O8 C17 C18 108.8(10) . . ?
O9 C18 C17 107.0(11) . . ?
O9 C19 C20 108.4(10) . . ?
O10 C20 C19 110.4(10) . . ?
O10 C21 C22 108.4(11) . . ?
O11 C22 C21 106.3(11) . . ?
O11 C23 C24 105.8(10) . . ?
O12 C24 C23 109.8(10) . . ?
C26 C25 N1 104.2(13) . . ?
C28 C27 N2 116.9(14) . . ?
C2 O1 C3 112.1(9) . . ?
C5 O2 C4 112.8(10) . . ?
C7 O3 C6 112.0(9) . . ?
C9 O4 C8 112.7(9) . . ?
C11 O5 C10 110.7(11) . . ?
C12 O6 C1 112.0(9) . . ?
C14 O7 C15 111.3(9) . . ?
C16 O8 C17 110.7(10) . . ?
C18 O9 C19 112.1(10) . . ?
C21 O10 C20 111.0(10) . . ?
C22 O11 C23 109.6(11) . . ?
C13 O12 C24 112.0(9) . . ?
O27 Cr1 O25 110.9(9) . . ?
O27 Cr1 O26 110.9(11) . . ?
O25 Cr1 O26 111.7(6) . . ?
O27 Cr1 Br1 107.2(6) . . ?
O25 Cr1 Br1 108.4(4) . . ?
O26 Cr1 Br1 107.5(8) . . ?
O30 Cr2 O29 115.0(17) . . ?
O30 Cr2 O28 112.6(15) . . ?
O29 Cr2 O28 112.0(8) . . ?
O30 Cr2 Br2 105.7(10) . . ?
O29 Cr2 Br2 101.8(12) . . ?
O28 Cr2 Br2 108.8(5) . . ?
O28 Cr2' O30' 116.6(11) . . ?
O28 Cr2' O29' 105.5(12) . . ?
O30' Cr2' O29' 111.5(17) . . ?
O28 Cr2' Br2 107.4(6) . . ?
O30' Cr2' Br2 108.8(13) . . ?
O29' Cr2' Br2 106.6(8) . . ?

_refine_diff_density_max         0.655
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.103


####################################################################### 
# 
# 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_1-296K
_database_code_depnum_ccdc_archive 'CCDC 1531725'
_audit_update_record             
;
2017-02-08 deposited with the CCDC.	2021-06-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H32 Br Cr N O9'
_chemical_formula_weight         490.31

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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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'

_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                   8.417(4)
_cell_length_b                   11.396(5)
_cell_length_c                   23.622(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2265.9(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2784
_cell_measurement_theta_min      2.57
_cell_measurement_theta_max      21.62

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_F_000             1016
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_absorpt_coefficient_mu    2.308
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6005
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12211
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.569
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             2324
_reflns_number_gt                1489
_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 SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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)+(0.0858P)²+1.9777P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.0070(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2324
_refine_ls_number_parameters     152
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0569
_refine_ls_wR_factor_ref         0.1825
_refine_ls_wR_factor_gt          0.1587
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.092
_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_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 0.56383(15) 0.77751(19) 0.59532(6) 0.0866(10) Uani 0.5 1 d . . P A -1
Br1 Br 0.59476(12) 0.7500 0.69032(3) 0.1322(5) Uani 1 2 d S T P . .
C1 C -0.1555(5) 0.1460(4) 0.52470(17) 0.0807(13) Uani 1 1 d . . . . .
H1A H -0.0619 0.1437 0.5007 0.097 Uiso 1 1 d R U . . .
H1B H -0.2486 0.1462 0.5005 0.097 Uiso 1 1 d R U . . .
C2 C -0.1568(5) 0.0425(4) 0.56207(19) 0.0771(12) Uani 1 1 d . . . . .
H2A H -0.2407 0.0502 0.5900 0.093 Uiso 1 1 d R U . . .
H2B H -0.1769 -0.0275 0.5399 0.093 Uiso 1 1 d R U . . .
C3 C 0.0013(5) -0.0648(3) 0.62702(15) 0.0685(10) Uani 1 1 d . . . . .
H3A H -0.0070 -0.1369 0.6054 0.082 Uiso 1 1 d R U . . .
H3B H -0.0862 -0.0620 0.6537 0.082 Uiso 1 1 d R U . . .
C4 C 0.1531(6) -0.0629(4) 0.65779(17) 0.0736(11) Uani 1 1 d . . . . .
H4A H 0.1646 -0.1328 0.6809 0.088 Uiso 1 1 d R U . . .
H4B H 0.2405 -0.0605 0.6310 0.088 Uiso 1 1 d R U . . .
C5 C 0.2950(5) 0.0417(4) 0.72861(19) 0.0795(12) Uani 1 1 d . . . . .
H5A H 0.3906 0.0456 0.7058 0.095 Uiso 1 1 d R U . . .
H5B H 0.2996 -0.0289 0.7515 0.095 Uiso 1 1 d R U . . .
C6 C 0.2832(5) 0.1460(4) 0.76610(16) 0.0749(11) Uani 1 1 d . . . . .
H6A H 0.1830 0.1453 0.7863 0.090 Uiso 1 1 d R U . . .
H6B H 0.3685 0.1446 0.7937 0.090 Uiso 1 1 d R U . . .
O1 O -0.1513(4) 0.2500 0.55781(13) 0.0602(9) Uani 1 2 d S T P . .
O2 O -0.0070(3) 0.0335(2) 0.59011(10) 0.0646(7) Uani 1 1 d . . . . .
O3 O 0.1589(3) 0.0379(2) 0.69318(9) 0.0613(7) Uani 1 1 d . . . . .
O4 O 0.2944(4) 0.2500 0.73271(14) 0.0615(9) Uani 1 2 d S T P . .
O5 O 0.7304(5) 0.7500 0.56476(19) 0.0932(13) Uani 1 2 d S T P . .
O6 O 0.4976(11) 0.8949(9) 0.5811(5) 0.145(3) Uani 0.5 1 d . U P A -1
O6' O 0.4291(12) 0.8047(10) 0.5759(4) 0.157(4) Uani 0.5 1 d . U P A -1
N1 N 0.1583(5) 0.235(3) 0.61860(18) 0.043(4) Uani 0.5 1 d . . P B -1
H1C H 0.0819 0.1826 0.6120 0.065 Uiso 0.5 1 calc R U P B -1
H1D H 0.1961 0.2247 0.6534 0.065 Uiso 0.5 1 calc R U P B -1
H1E H 0.1189 0.3070 0.6153 0.065 Uiso 0.5 1 calc R U P B -1
C7 C 0.2878(10) 0.2186(8) 0.5771(3) 0.080(4) Uani 0.5 1 d . . P B -1
H7A H 0.3271 0.1388 0.5804 0.097 Uiso 0.5 1 calc R U P B -1
H7B H 0.2440 0.2275 0.5394 0.097 Uiso 0.5 1 calc R U P B -1
C8 C 0.4214(12) 0.2987(11) 0.5831(6) 0.135(6) Uani 0.5 1 d . . P B -1
H8A H 0.4993 0.2818 0.5545 0.203 Uiso 0.5 1 calc R U P B -1
H8B H 0.3849 0.3780 0.5787 0.203 Uiso 0.5 1 calc R U P B -1
H8C H 0.4682 0.2892 0.6198 0.203 Uiso 0.5 1 calc R U P B -1


_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 O6' 1.262(9) . ?
Cr1 O6 1.488(9) . ?
Cr1 O5 1.608(5) . ?
Cr1 Br1 2.281(2) . ?
C1 O1 1.420(4) . ?
C1 C2 1.473(6) . ?
C2 O2 1.428(4) . ?
C3 O2 1.421(4) . ?
C3 C4 1.470(6) . ?
C4 O3 1.421(4) . ?
C5 O3 1.420(4) . ?
C5 C6 1.486(6) . ?
C6 O4 1.427(4) . ?
O1 C1 1.420(4) 7_565 ?
O4 C6 1.427(4) 7_565 ?
O6 O6' 1.185(12) . ?
N1 C7 1.477(9) . ?
C7 C8 1.456(13) . ?

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
O6' Cr1 O6 50.2(5) . . ?
O6' Cr1 O5 131.9(5) . . ?
O6 Cr1 O5 113.6(4) . . ?
O6' Cr1 Br1 119.6(5) . . ?
O6 Cr1 Br1 112.9(5) . . ?
O5 Cr1 Br1 108.38(17) . . ?
O1 C1 C2 109.8(3) . . ?
O2 C2 C1 109.2(3) . . ?
O2 C3 C4 109.6(3) . . ?
O3 C4 C3 109.4(3) . . ?
O3 C5 C6 108.8(3) . . ?
O4 C6 C5 109.3(3) . . ?
C1 O1 C1 113.1(4) . 7_565 ?
C3 O2 C2 112.7(3) . . ?
C5 O3 C4 113.5(3) . . ?
C6 O4 C6 112.3(4) 7_565 . ?
O6' O6 Cr1 54.9(6) . . ?
O6 O6' Cr1 74.8(8) . . ?
C8 C7 N1 115.3(11) . . ?

_refine_diff_density_max         0.696
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.057





####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 2078366'
loop_
_audit_author_name
_audit_author_address
'Zi-Yi Du'
;Jiangxi normal university
China
;
_audit_update_record             
;
2021-04-18 deposited with the CCDC.	2021-06-23 downloaded from the CCDC.
;
_vrf_PLAT201_2                   
;
PROBLEM:  
  Isotropic non-H Atoms in Main Residue(s) .......         18 Report
              O1'       O2'       O3'       O4'       O5'                 etc.   
                
RESPONSE: 
 Due to the serious orientational disorder of the 18-crown-6
molecule, the atoms of 18-crown-6 are refined isotropically.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H31 Br2 Cr N O9'
_chemical_formula_weight         569.22

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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   8.6959(3)
_cell_length_b                   11.6717(5)
_cell_length_c                   12.2829(5)
_cell_angle_alpha                109.137(4)
_cell_angle_beta                 98.956(3)
_cell_angle_gamma                98.155(3)
_cell_volume                     1138.29(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    6850
_cell_measurement_theta_min      3.9520
_cell_measurement_theta_max      25.4160

_exptl_crystal_description       column
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.054
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            20109
_diffrn_reflns_av_unetI/netI     0.0471
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.316
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             4465
_reflns_number_gt                3214
_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 FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0561P)²+1.6594P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4465
_refine_ls_number_parameters     245
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0567
_refine_ls_wR_factor_ref         0.1464
_refine_ls_wR_factor_gt          0.1331
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.065
_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 1.06853(10) 0.84458(8) 0.66610(8) 0.0516(3) Uani 1 1 d . . . . .
Br1 Br 1.00712(9) 0.86013(7) 0.84748(6) 0.0838(3) Uani 1 1 d . . . . .
Br2 Br 0.56575(7) 0.85925(5) 0.55258(5) 0.0600(2) Uani 1 1 d . . . . .
N1 N 0.5593(5) 0.7000(4) 0.2740(3) 0.0428(9) Uani 1 1 d D . . . .
H1C H 0.576(13) 0.655(7) 0.204(4) 0.064 Uiso 0.5 1 d D U P . .
H1D H 0.513(11) 0.650(7) 0.306(9) 0.064 Uiso 0.5 1 d D U P . .
H1E H 0.495(8) 0.748(7) 0.260(7) 0.064 Uiso 0.5 1 d D U P . .
H1C' H 0.580(12) 0.629(5) 0.230(6) 0.064 Uiso 0.5 1 d D U P . .
H1D' H 0.488(10) 0.680(9) 0.314(9) 0.064 Uiso 0.5 1 d D U P . .
H1E' H 0.507(10) 0.734(8) 0.227(5) 0.064 Uiso 0.5 1 d D U P . .
C13 C 0.7097(6) 0.7778(5) 0.3551(5) 0.0576(14) Uani 1 1 d . . . . .
H13A H 0.7589 0.7296 0.3961 0.069 Uiso 1 1 calc R U . . .
H13B H 0.7818 0.7998 0.3089 0.069 Uiso 1 1 calc R U . . .
C14 C 0.6883(7) 0.8928(5) 0.4434(5) 0.0567(14) Uani 1 1 d . . . . .
H14A H 0.6347 0.9395 0.4028 0.068 Uiso 1 1 calc R U . . .
H14B H 0.7919 0.9434 0.4873 0.068 Uiso 1 1 calc R U . . .
O7 O 1.2506(5) 0.8366(4) 0.6757(5) 0.0876(14) Uani 1 1 d . . . . .
O8 O 0.9566(6) 0.7233(4) 0.5679(4) 0.0859(14) Uani 1 1 d . . . . .
O9 O 1.0390(5) 0.9671(4) 0.6434(4) 0.0833(13) Uani 1 1 d . . . . .
C1 C 0.689(2) 0.4346(17) 0.3010(17) 0.089(5) Uiso 0.441(7) 1 d . . P A 1
H1A H 0.7536 0.5030 0.3689 0.107 Uiso 0.441(7) 1 calc R U P A 1
H1B H 0.7398 0.3640 0.2875 0.107 Uiso 0.441(7) 1 calc R U P A 1
C2 C 0.514(2) 0.3999(14) 0.3215(14) 0.062(4) Uiso 0.441(7) 1 d . . P A 1
H2A H 0.4481 0.3340 0.2520 0.074 Uiso 0.441(7) 1 calc R U P A 1
H2B H 0.5183 0.3724 0.3881 0.074 Uiso 0.441(7) 1 calc R U P A 1
C3 C 0.291(2) 0.4680(15) 0.3464(14) 0.072(4) Uiso 0.441(7) 1 d . . P A 1
H3A H 0.2823 0.4267 0.4028 0.087 Uiso 0.441(7) 1 calc R U P A 1
H3B H 0.2316 0.4107 0.2696 0.087 Uiso 0.441(7) 1 calc R U P A 1
C4 C 0.2170(19) 0.5816(18) 0.3816(15) 0.071(4) Uiso 0.441(7) 1 d . . P A 1
H4A H 0.1072 0.5582 0.3859 0.085 Uiso 0.441(7) 1 calc R U P A 1
H4B H 0.2752 0.6405 0.4581 0.085 Uiso 0.441(7) 1 calc R U P A 1
C5 C 0.169(2) 0.7419(17) 0.3336(17) 0.082(5) Uiso 0.441(7) 1 d . . P A 1
H5A H 0.2370 0.7986 0.4077 0.098 Uiso 0.441(7) 1 calc R U P A 1
H5B H 0.0623 0.7246 0.3457 0.098 Uiso 0.441(7) 1 calc R U P A 1
C6 C 0.1700(16) 0.8026(13) 0.2366(16) 0.060(4) Uiso 0.441(7) 1 d . . P A 1
H6A H 0.0993 0.7469 0.1634 0.071 Uiso 0.441(7) 1 calc R U P A 1
H6B H 0.1314 0.8791 0.2617 0.071 Uiso 0.441(7) 1 calc R U P A 1
C7 C 0.310(3) 0.878(2) 0.132(2) 0.107(6) Uiso 0.441(7) 1 d . . P A 1
H7A H 0.2730 0.9552 0.1572 0.128 Uiso 0.441(7) 1 calc R U P A 1
H7B H 0.2377 0.8218 0.0597 0.128 Uiso 0.441(7) 1 calc R U P A 1
C8 C 0.490(3) 0.9037(14) 0.1091(14) 0.072(4) Uiso 0.441(7) 1 d . . P A 1
H8A H 0.4906 0.9417 0.0497 0.086 Uiso 0.441(7) 1 calc R U P A 1
H8B H 0.5617 0.9601 0.1815 0.086 Uiso 0.441(7) 1 calc R U P A 1
C9 C 0.690(2) 0.8087(18) 0.0444(17) 0.089(5) Uiso 0.441(7) 1 d . . P A 1
H9A H 0.7688 0.8640 0.1135 0.107 Uiso 0.441(7) 1 calc R U P A 1
H9B H 0.6883 0.8441 -0.0169 0.107 Uiso 0.441(7) 1 calc R U P A 1
C10 C 0.7349(15) 0.6793(16) 0.0011(12) 0.053(3) Uiso 0.441(7) 1 d . . P A 1
H10A H 0.6538 0.6231 -0.0661 0.064 Uiso 0.441(7) 1 calc R U P A 1
H10B H 0.8352 0.6868 -0.0239 0.064 Uiso 0.441(7) 1 calc R U P A 1
C11 C 0.7664(19) 0.5075(16) 0.0440(16) 0.079(4) Uiso 0.441(7) 1 d . . P A 1
H11A H 0.8577 0.5025 0.0076 0.094 Uiso 0.441(7) 1 calc R U P A 1
H11B H 0.6727 0.4563 -0.0151 0.094 Uiso 0.441(7) 1 calc R U P A 1
C12 C 0.791(2) 0.4601(16) 0.1493(19) 0.075(5) Uiso 0.441(7) 1 d . . P A 1
H12A H 0.8020 0.3745 0.1215 0.089 Uiso 0.441(7) 1 calc R U P A 1
H12B H 0.8859 0.5097 0.2076 0.089 Uiso 0.441(7) 1 calc R U P A 1
O1 O 0.6653(15) 0.4698(10) 0.1961(10) 0.078(3) Uiso 0.441(7) 1 d . . P A 1
O2 O 0.4568(13) 0.4981(9) 0.3418(8) 0.065(3) Uiso 0.441(7) 1 d . . P A 1
O3 O 0.2251(11) 0.6321(9) 0.2972(9) 0.062(3) Uiso 0.441(7) 1 d . . P A 1
O4 O 0.3177(14) 0.8264(10) 0.2189(10) 0.071(3) Uiso 0.441(7) 1 d D . P A 1
O5 O 0.5388(15) 0.7960(12) 0.0727(10) 0.073(3) Uiso 0.441(7) 1 d . . P A 1
O6 O 0.7475(10) 0.6344(9) 0.0877(9) 0.058(2) Uiso 0.441(7) 1 d . . P A 1
C1' C 0.585(2) 0.4135(14) 0.3230(12) 0.076(4) Uiso 0.559(7) 1 d . . P A 2
H1'A H 0.6532 0.4785 0.3921 0.092 Uiso 0.559(7) 1 calc R U P A 2
H1'B H 0.6155 0.3356 0.3181 0.092 Uiso 0.559(7) 1 calc R U P A 2
C2' C 0.4018(17) 0.4057(12) 0.3336(12) 0.080(4) Uiso 0.559(7) 1 d . . P A 2
H2'A H 0.3322 0.3444 0.2627 0.096 Uiso 0.559(7) 1 calc R U P A 2
H2'B H 0.3848 0.3831 0.4007 0.096 Uiso 0.559(7) 1 calc R U P A 2
C3' C 0.2100(14) 0.5131(13) 0.3444(11) 0.062(3) Uiso 0.559(7) 1 d . . P A 2
H3'A H 0.1822 0.4834 0.4053 0.075 Uiso 0.559(7) 1 calc R U P A 2
H3'B H 0.1502 0.4541 0.2685 0.075 Uiso 0.559(7) 1 calc R U P A 2
C4' C 0.1665(14) 0.6391(11) 0.3633(11) 0.065(3) Uiso 0.559(7) 1 d . . P A 2
H4'A H 0.0544 0.6331 0.3644 0.077 Uiso 0.559(7) 1 calc R U P A 2
H4'B H 0.2276 0.6989 0.4384 0.077 Uiso 0.559(7) 1 calc R U P A 2
C5' C 0.1694(13) 0.7919(10) 0.2932(12) 0.059(3) Uiso 0.559(7) 1 d . . P A 2
H5'A H 0.2366 0.8483 0.3677 0.070 Uiso 0.559(7) 1 calc R U P A 2
H5'B H 0.0592 0.7902 0.2991 0.070 Uiso 0.559(7) 1 calc R U P A 2
C6' C 0.2021(14) 0.8368(11) 0.1921(11) 0.066(3) Uiso 0.559(7) 1 d . . P A 2
H6'A H 0.1382 0.7787 0.1172 0.079 Uiso 0.559(7) 1 calc R U P A 2
H6'B H 0.1746 0.9171 0.2046 0.079 Uiso 0.559(7) 1 calc R U P A 2
C7' C 0.4011(18) 0.8985(11) 0.1112(10) 0.062(3) Uiso 0.559(7) 1 d . . P A 2
H7'A H 0.3891 0.9840 0.1376 0.074 Uiso 0.559(7) 1 calc R U P A 2
H7'B H 0.3299 0.8540 0.0349 0.074 Uiso 0.559(7) 1 calc R U P A 2
C8' C 0.5813(18) 0.8918(13) 0.1015(13) 0.084(4) Uiso 0.559(7) 1 d . . P A 2
H8'A H 0.6105 0.9272 0.0445 0.100 Uiso 0.559(7) 1 calc R U P A 2
H8'B H 0.6527 0.9383 0.1774 0.100 Uiso 0.559(7) 1 calc R U P A 2
C9' C 0.7384(13) 0.7528(13) 0.0371(11) 0.059(3) Uiso 0.559(7) 1 d . . P A 2
H9'A H 0.8235 0.8068 0.1025 0.071 Uiso 0.559(7) 1 calc R U P A 2
H9'B H 0.7469 0.7750 -0.0315 0.071 Uiso 0.559(7) 1 calc R U P A 2
C10' C 0.7514(17) 0.6151(14) 0.0106(15) 0.087(4) Uiso 0.559(7) 1 d . . P A 2
H10C H 0.6616 0.5615 -0.0510 0.105 Uiso 0.559(7) 1 calc R U P A 2
H10D H 0.8479 0.6017 -0.0176 0.105 Uiso 0.559(7) 1 calc R U P A 2
C11' C 0.7675(15) 0.4645(11) 0.0934(13) 0.066(3) Uiso 0.559(7) 1 d . . P A 2
H11C H 0.8697 0.4532 0.0742 0.080 Uiso 0.559(7) 1 calc R U P A 2
H11D H 0.6848 0.4091 0.0268 0.080 Uiso 0.559(7) 1 calc R U P A 2
C12' C 0.753(2) 0.4309(16) 0.2053(16) 0.104(5) Uiso 0.559(7) 1 d . . P A 2
H12C H 0.7700 0.3477 0.1929 0.125 Uiso 0.559(7) 1 calc R U P A 2
H12D H 0.8313 0.4884 0.2734 0.125 Uiso 0.559(7) 1 calc R U P A 2
O1' O 0.6010(10) 0.4385(7) 0.2234(8) 0.071(2) Uiso 0.559(7) 1 d . . P A 2
O2' O 0.3718(10) 0.5220(7) 0.3481(6) 0.0595(19) Uiso 0.559(7) 1 d . . P A 2
O3' O 0.1999(8) 0.6781(7) 0.2706(6) 0.0524(18) Uiso 0.559(7) 1 d . . P A 2
O4' O 0.3662(9) 0.8453(7) 0.1910(7) 0.057(2) Uiso 0.559(7) 1 d D . P A 2
O5' O 0.5933(11) 0.7657(8) 0.0653(7) 0.065(2) Uiso 0.559(7) 1 d . . P A 2
O6' O 0.7538(9) 0.5849(9) 0.1119(8) 0.072(2) Uiso 0.559(7) 1 d . . P A 2


_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 O7 1.588(4) . ?
Cr1 O8 1.591(4) . ?
Cr1 O9 1.592(4) . ?
Cr1 Br1 2.3268(10) . ?
Br2 C14 1.939(5) . ?
N1 C13 1.481(6) . ?
C13 C14 1.480(7) . ?
C1 O1 1.47(2) . ?
C1 C2 1.60(2) . ?
C2 O2 1.278(17) . ?
C3 O2 1.450(19) . ?
C3 C4 1.52(2) . ?
C4 O3 1.356(18) . ?
C5 O3 1.39(2) . ?
C5 C6 1.57(2) . ?
C6 O4 1.342(18) . ?
C7 O4 1.39(2) . ?
C7 C8 1.63(2) . ?
C8 O5 1.34(2) . ?
C9 O5 1.41(2) . ?
C9 C10 1.56(2) . ?
C10 O6 1.329(17) . ?
C11 O6 1.44(2) . ?
C11 C12 1.56(2) . ?
C12 O1 1.31(2) . ?
C1' O1' 1.370(16) . ?
C1' C2' 1.610(19) . ?
C2' O2' 1.377(15) . ?
C3' O2' 1.388(14) . ?
C3' C4' 1.524(17) . ?
C4' O3' 1.411(14) . ?
C5' O3' 1.340(13) . ?
C5' C6' 1.546(16) . ?
C6' O4' 1.419(15) . ?
C7' O4' 1.370(15) . ?
C7' C8' 1.601(17) . ?
C8' O5' 1.415(17) . ?
C9' O5' 1.375(14) . ?
C9' C10' 1.556(18) . ?
C10' O6' 1.399(18) . ?
C11' O6' 1.373(15) . ?
C11' C12' 1.57(2) . ?
C12' O1' 1.382(19) . ?

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
O7 Cr1 O8 111.2(3) . . ?
O7 Cr1 O9 110.6(2) . . ?
O8 Cr1 O9 111.9(3) . . ?
O7 Cr1 Br1 107.76(19) . . ?
O8 Cr1 Br1 108.35(17) . . ?
O9 Cr1 Br1 106.82(18) . . ?
C14 C13 N1 113.6(4) . . ?
C13 C14 Br2 112.3(4) . . ?
O1 C1 C2 105.0(14) . . ?
O2 C2 C1 106.8(13) . . ?
O2 C3 C4 112.7(14) . . ?
O3 C4 C3 106.6(14) . . ?
O3 C5 C6 109.4(14) . . ?
O4 C6 C5 110.2(12) . . ?
O4 C7 C8 107.0(16) . . ?
O5 C8 C7 109.5(14) . . ?
O5 C9 C10 109.5(15) . . ?
O6 C10 C9 109.8(13) . . ?
O6 C11 C12 108.9(14) . . ?
O1 C12 C11 107.6(15) . . ?
C12 O1 C1 109.3(15) . . ?
C2 O2 C3 109.1(12) . . ?
C4 O3 C5 107.0(14) . . ?
C6 O4 C7 107.6(15) . . ?
C8 O5 C9 113.2(15) . . ?
C10 O6 C11 110.3(14) . . ?
O1' C1' C2' 108.4(11) . . ?
O2' C2' C1' 106.1(10) . . ?
O2' C3' C4' 110.4(10) . . ?
O3' C4' C3' 108.9(10) . . ?
O3' C5' C6' 108.9(10) . . ?
O4' C6' C5' 108.2(10) . . ?
O4' C7' C8' 107.3(10) . . ?
O5' C8' C7' 108.0(11) . . ?
O5' C9' C10' 108.0(10) . . ?
O6' C10' C9' 110.7(12) . . ?
O6' C11' C12' 111.2(11) . . ?
O1' C12' C11' 107.3(13) . . ?
C1' O1' C12' 109.1(11) . . ?
C2' O2' C3' 106.7(10) . . ?
C5' O3' C4' 107.5(9) . . ?
C7' O4' C6' 108.9(10) . . ?
C9' O5' C8' 110.3(11) . . ?
C11' O6' C10' 112.9(12) . . ?

_refine_diff_density_max         0.654
_refine_diff_density_min         -0.652
_refine_diff_density_rms         0.089

_shelxl_version_number           2014-3



####################################################################### 
# 
# 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_2_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2078367'
loop_
_audit_author_name
_audit_author_address
'Zi-Yi Du'
;Jiangxi normal university
China
;
_audit_update_record             
;
2021-04-18 deposited with the CCDC.	2021-06-23 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C14 H31 Br2 Cr N O9'
_chemical_formula_weight         569.22

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'
N N 0.0061 0.0033 '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'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   8.7327(3)
_cell_length_b                   11.6396(4)
_cell_length_c                   12.0019(4)
_cell_angle_alpha                107.718(2)
_cell_angle_beta                 100.411(2)
_cell_angle_gamma                98.142(2)
_cell_volume                     1117.48(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9958
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      26.38

_exptl_crystal_description       column
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_F_000             576
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    4.129
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28058
_diffrn_reflns_av_unetI/netI     0.0187
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.135
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             4397
_reflns_number_gt                3886
_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 SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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)+(0.0286P)²+0.2551P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0013(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4397
_refine_ls_number_parameters     254
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0210
_refine_ls_wR_factor_ref         0.0538
_refine_ls_wR_factor_gt          0.0522
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.002
_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 1.06717(4) 0.84767(3) 0.66893(3) 0.03396(9) Uani 1 1 d . . . . .
Br1 Br 1.01562(3) 0.86085(2) 0.85715(2) 0.04769(8) Uani 1 1 d . . . . .
Br2 Br 0.55124(2) 0.85939(2) 0.55157(2) 0.03756(7) Uani 1 1 d . . . . .
N1 N 0.54557(19) 0.69107(15) 0.27407(15) 0.0329(3) Uani 1 1 d D . . . .
H1C H 0.568(3) 0.6344(15) 0.2147(15) 0.049 Uiso 1 1 d D U . . .
H1D H 0.479(2) 0.6530(18) 0.3070(18) 0.049 Uiso 1 1 d D U . . .
H1E H 0.491(2) 0.7377(17) 0.2426(18) 0.049 Uiso 1 1 d D U . . .
C1 C 0.7507(3) 0.4515(2) 0.0941(2) 0.0481(5) Uani 1 1 d . . . . .
H1A H 0.8533 0.4371 0.0746 0.058 Uiso 1 1 calc R U . . .
H1B H 0.6635 0.3984 0.0246 0.058 Uiso 1 1 calc R U . . .
C2 C 0.7352(3) 0.4194(2) 0.2041(2) 0.0469(5) Uani 1 1 d . . . . .
H2A H 0.7464 0.3332 0.1917 0.056 Uiso 1 1 calc R U . . .
H2B H 0.8196 0.4745 0.2745 0.056 Uiso 1 1 calc R U . . .
C3 C 0.5585(3) 0.4066(2) 0.3291(2) 0.0458(5) Uani 1 1 d . . . . .
H3A H 0.6260 0.4721 0.4025 0.055 Uiso 1 1 calc R U . . .
H3B H 0.5881 0.3272 0.3272 0.055 Uiso 1 1 calc R U . . .
C4 C 0.3876(3) 0.39942(19) 0.3312(2) 0.0456(5) Uani 1 1 d . . . . .
H4A H 0.3200 0.3398 0.2543 0.055 Uiso 1 1 calc R U . . .
H4B H 0.3657 0.3704 0.3974 0.055 Uiso 1 1 calc R U . . .
C5 C 0.1838(2) 0.51329(19) 0.3362(2) 0.0410(5) Uani 1 1 d . . . . .
H5A H 0.1460 0.4779 0.3941 0.049 Uiso 1 1 calc R U . . .
H5B H 0.1248 0.4601 0.2537 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1550(2) 0.64133(19) 0.36020(19) 0.0400(5) Uani 1 1 d . . . . .
H6A H 0.0418 0.6412 0.3609 0.048 Uiso 1 1 calc R U . . .
H6B H 0.2214 0.6962 0.4398 0.048 Uiso 1 1 calc R U . . .
C7 C 0.1745(2) 0.80846(18) 0.2898(2) 0.0421(5) Uani 1 1 d . . . . .
H7A H 0.2470 0.8632 0.3671 0.050 Uiso 1 1 calc R U . . .
H7B H 0.0637 0.8131 0.2954 0.050 Uiso 1 1 calc R U . . .
C8 C 0.2107(3) 0.8493(2) 0.1893(2) 0.0443(5) Uani 1 1 d . . . . .
H8A H 0.1429 0.7915 0.1114 0.053 Uiso 1 1 calc R U . . .
H8B H 0.1882 0.9324 0.1998 0.053 Uiso 1 1 calc R U . . .
C9 C 0.4233(3) 0.9036(2) 0.1053(2) 0.0491(5) Uani 1 1 d . . . . .
H9A H 0.4153 0.9913 0.1282 0.059 Uiso 1 1 calc R U . . .
H9B H 0.3535 0.8589 0.0240 0.059 Uiso 1 1 calc R U . . .
C10 C 0.5915(3) 0.8931(2) 0.1044(2) 0.0481(5) Uani 1 1 d . . . . .
H10A H 0.6292 0.9321 0.0488 0.058 Uiso 1 1 calc R U . . .
H10B H 0.6608 0.9363 0.1861 0.058 Uiso 1 1 calc R U . . .
C11 C 0.7514(3) 0.7486(2) 0.0462(2) 0.0494(5) Uani 1 1 d . . . . .
H11A H 0.8355 0.7969 0.1196 0.059 Uiso 1 1 calc R U . . .
H11B H 0.7720 0.7775 -0.0203 0.059 Uiso 1 1 calc R U . . .
C12 C 0.7544(3) 0.6147(2) 0.0146(2) 0.0499(5) Uani 1 1 d . . . . .
H12A H 0.6640 0.5658 -0.0542 0.060 Uiso 1 1 calc R U . . .
H12B H 0.8545 0.5998 -0.0093 0.060 Uiso 1 1 calc R U . . .
C13 C 0.6993(2) 0.76518(18) 0.35722(18) 0.0368(4) Uani 1 1 d . . . . .
H13A H 0.7747 0.7828 0.3091 0.044 Uiso 1 1 calc R U . . .
H13B H 0.7447 0.7158 0.4038 0.044 Uiso 1 1 calc R U . . .
C14 C 0.6840(2) 0.88530(18) 0.44358(18) 0.0366(4) Uani 1 1 d . . . . .
H14A H 0.6371 0.9345 0.3974 0.044 Uiso 1 1 calc R U . . .
H14B H 0.7912 0.9329 0.4917 0.044 Uiso 1 1 calc R U . . .
O1 O 0.58309(16) 0.43367(12) 0.22470(13) 0.0390(3) Uani 1 1 d . . . . .
O2 O 0.35088(16) 0.51857(12) 0.34861(13) 0.0378(3) Uani 1 1 d . . . . .
O3 O 0.19473(16) 0.68502(12) 0.26791(13) 0.0383(3) Uani 1 1 d . . . . .
O4 O 0.37421(17) 0.85192(13) 0.18967(13) 0.0408(3) Uani 1 1 d . . . . .
O5 O 0.59951(17) 0.76613(13) 0.06626(13) 0.0422(3) Uani 1 1 d . . . . .
O6 O 0.74350(17) 0.57772(13) 0.11613(13) 0.0428(3) Uani 1 1 d . . . . .
O7 O 1.24926(18) 0.83495(14) 0.67719(15) 0.0475(4) Uani 1 1 d . . . . .
O8 O 0.94605(18) 0.72878(14) 0.56957(13) 0.0474(4) Uani 1 1 d . . . . .
O9 O 1.03995(19) 0.97339(14) 0.64701(15) 0.0486(4) 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 O9 1.6054(14) . ?
Cr1 O7 1.6059(15) . ?
Cr1 O8 1.6066(15) . ?
Cr1 Br1 2.3464(4) . ?
Br2 C14 1.9487(19) . ?
N1 C13 1.485(2) . ?
C1 O6 1.425(3) . ?
C1 C2 1.500(3) . ?
C2 O1 1.417(2) . ?
C3 O1 1.426(3) . ?
C3 C4 1.488(3) . ?
C4 O2 1.430(2) . ?
C5 O2 1.430(2) . ?
C5 C6 1.496(3) . ?
C6 O3 1.427(2) . ?
C7 O3 1.422(2) . ?
C7 C8 1.492(3) . ?
C8 O4 1.423(3) . ?
C9 O4 1.423(3) . ?
C9 C10 1.492(3) . ?
C10 O5 1.424(3) . ?
C11 O5 1.422(3) . ?
C11 C12 1.492(3) . ?
C12 O6 1.424(3) . ?
C13 C14 1.506(3) . ?

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
O9 Cr1 O7 111.18(8) . . ?
O9 Cr1 O8 112.05(8) . . ?
O7 Cr1 O8 111.75(8) . . ?
O9 Cr1 Br1 106.70(6) . . ?
O7 Cr1 Br1 107.01(6) . . ?
O8 Cr1 Br1 107.82(6) . . ?
O6 C1 C2 109.25(17) . . ?
O1 C2 C1 108.14(17) . . ?
O1 C3 C4 108.78(17) . . ?
O2 C4 C3 109.48(17) . . ?
O2 C5 C6 108.54(16) . . ?
O3 C6 C5 108.73(16) . . ?
O3 C7 C8 109.06(17) . . ?
O4 C8 C7 108.79(17) . . ?
O4 C9 C10 108.81(17) . . ?
O5 C10 C9 109.12(17) . . ?
O5 C11 C12 109.04(17) . . ?
O6 C12 C11 109.34(18) . . ?
N1 C13 C14 113.38(16) . . ?
C13 C14 Br2 111.85(14) . . ?
C2 O1 C3 112.07(16) . . ?
C4 O2 C5 111.49(15) . . ?
C7 O3 C6 110.52(15) . . ?
C9 O4 C8 112.41(16) . . ?
C11 O5 C10 112.08(16) . . ?
C12 O6 C1 112.63(16) . . ?

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.047

_shelxl_version_number           2014-3



