# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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
_database_code_depnum_ccdc_archive 'CCDC 1038142'
_audit_update_record             
;
2015-03-06 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 Cr Mn N O12'
_chemical_formula_weight         423.14

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   8.2865(12)
_cell_length_b                   8.2865(12)
_cell_length_c                   13.880(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     825.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7943
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.4

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             428
_exptl_absorpt_coefficient_mu    1.481
_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      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8208
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.20
_diffrn_reflns_theta_max         27.42
_reflns_number_total             638
_reflns_number_gt                611
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL

_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)+(0.0291P)²+1.1025P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         638
_refine_ls_number_parameters     40
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0817
_refine_ls_wR_factor_gt          0.0805
_refine_ls_goodness_of_fit_ref   1.234
_refine_ls_restrained_S_all      1.276
_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
Mn1 Mn 0.3333 0.6667 0.2500 0.0166(2) Uani 1 6 d S . .
Cr1 Cr 0.0000 0.0000 0.0000 0.0132(2) Uani 1 6 d S . .
O2 O 0.3386(3) 0.4496(3) 0.16470(14) 0.0368(5) Uani 1 1 d . . .
O1 O 0.2031(2) 0.1893(2) 0.08085(13) 0.0250(4) Uani 1 1 d . . .
C1 C 0.2092(4) 0.3307(4) 0.11665(18) 0.0296(6) Uani 1 1 d . . .
H1A H 0.1075 0.3471 0.1061 0.035 Uiso 1 1 calc R . .
C2 C 0.6667 0.3333 0.1603(17) 0.177(8) Uani 1 3 d S . .
H3 H 0.7212 0.4542 0.1092 0.212 Uiso 1 1 d R . .
N1 N 0.562(3) 0.2809(17) 0.2500 0.108(6) Uani 0.33 2 d SPU . .
H2 H 0.4819 0.1492 0.2500 0.130 Uiso 0.33 1 d PR . .

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
Mn1 0.0148(3) 0.0148(3) 0.0201(4) 0.000 0.000 0.00740(14)
Cr1 0.0120(3) 0.0120(3) 0.0157(4) 0.000 0.000 0.00601(14)
O2 0.0310(10) 0.0324(11) 0.0472(11) -0.0225(9) -0.0121(9) 0.0159(9)
O1 0.0220(9) 0.0208(8) 0.0324(9) -0.0094(7) -0.0074(7) 0.0107(7)
C1 0.0263(13) 0.0253(12) 0.0389(14) -0.0115(11) -0.0073(11) 0.0142(11)
C2 0.089(6) 0.089(6) 0.35(3) 0.000 0.000 0.044(3)
N1 0.097(9) 0.073(7) 0.162(11) 0.029(8) 0.000 0.048(5)

_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
Mn1 O2 2.1722(18) 6_565 ?
Mn1 O2 2.1722(18) 3_565 ?
Mn1 O2 2.1722(18) 5 ?
Mn1 O2 2.1722(18) 2_665 ?
Mn1 O2 2.1722(18) . ?
Mn1 O2 2.1722(18) 4_665 ?
Cr1 O1 1.9781(16) . ?
Cr1 O1 1.9781(16) 7 ?
Cr1 O1 1.9781(16) 3 ?
Cr1 O1 1.9781(16) 2 ?
Cr1 O1 1.9781(16) 8 ?
Cr1 O1 1.9781(16) 9 ?
O2 C1 1.229(3) . ?
O1 C1 1.250(3) . ?
C1 H1A 0.9300 . ?
C2 N1 1.454(18) 2_655 ?
C2 N1 1.454(18) 3_665 ?
C2 N1 1.454(18) . ?
C2 H3 1.1217 . ?
N1 N1 1.30(4) 3_665 ?
N1 N1 1.30(4) 2_655 ?
N1 C2 1.454(18) 4_665 ?
N1 H2 0.9524 . ?

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
O2 Mn1 O2 88.37(12) 6_565 3_565 ?
O2 Mn1 O2 93.11(8) 6_565 5 ?
O2 Mn1 O2 85.44(11) 3_565 5 ?
O2 Mn1 O2 85.44(11) 6_565 2_665 ?
O2 Mn1 O2 93.11(8) 3_565 2_665 ?
O2 Mn1 O2 177.99(11) 5 2_665 ?
O2 Mn1 O2 177.99(11) 6_565 . ?
O2 Mn1 O2 93.11(8) 3_565 . ?
O2 Mn1 O2 88.37(12) 5 . ?
O2 Mn1 O2 93.11(8) 2_665 . ?
O2 Mn1 O2 93.11(8) 6_565 4_665 ?
O2 Mn1 O2 177.99(11) 3_565 4_665 ?
O2 Mn1 O2 93.11(8) 5 4_665 ?
O2 Mn1 O2 88.37(12) 2_665 4_665 ?
O2 Mn1 O2 85.44(11) . 4_665 ?
O1 Cr1 O1 180.00(13) . 7 ?
O1 Cr1 O1 90.98(7) . 3 ?
O1 Cr1 O1 89.02(7) 7 3 ?
O1 Cr1 O1 90.98(7) . 2 ?
O1 Cr1 O1 89.02(7) 7 2 ?
O1 Cr1 O1 90.98(7) 3 2 ?
O1 Cr1 O1 89.02(7) . 8 ?
O1 Cr1 O1 90.98(7) 7 8 ?
O1 Cr1 O1 89.02(7) 3 8 ?
O1 Cr1 O1 180.00(10) 2 8 ?
O1 Cr1 O1 89.02(7) . 9 ?
O1 Cr1 O1 90.98(7) 7 9 ?
O1 Cr1 O1 180.00(12) 3 9 ?
O1 Cr1 O1 89.02(7) 2 9 ?
O1 Cr1 O1 90.98(7) 8 9 ?
C1 O2 Mn1 126.09(18) . . ?
C1 O1 Cr1 126.01(16) . . ?
O2 C1 O1 125.3(2) . . ?
O2 C1 H1A 117.4 . . ?
O1 C1 H1A 117.4 . . ?
N1 C2 N1 53.2(19) 2_655 3_665 ?
N1 C2 N1 53.2(19) 2_655 . ?
N1 C2 N1 53.2(19) 3_665 . ?
N1 C2 H3 139.5 2_655 . ?
N1 C2 H3 98.1 3_665 . ?
N1 C2 H3 136.2 . . ?
N1 N1 N1 60.000(2) 3_665 2_655 ?
N1 N1 C2 63.4(9) 3_665 4_665 ?
N1 N1 C2 63.4(9) 2_655 4_665 ?
N1 N1 C2 63.4(9) 3_665 . ?
N1 N1 C2 63.4(9) 2_655 . ?
C2 N1 C2 118(2) 4_665 . ?
N1 N1 H2 157.0 3_665 . ?
N1 N1 H2 97.0 2_655 . ?
C2 N1 H2 108.1 4_665 . ?
C2 N1 H2 108.1 . . ?

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
O2 Mn1 O2 C1 -161.6(2) 6_565 . . . ?
O2 Mn1 O2 C1 -24.3(3) 3_565 . . . ?
O2 Mn1 O2 C1 61.1(2) 5 . . . ?
O2 Mn1 O2 C1 -117.5(2) 2_665 . . . ?
O2 Mn1 O2 C1 154.3(3) 4_665 . . . ?
O1 Cr1 O1 C1 -15.1(2) 7 . . . ?
O1 Cr1 O1 C1 -130.00(19) 3 . . . ?
O1 Cr1 O1 C1 -39.0(2) 2 . . . ?
O1 Cr1 O1 C1 141.0(2) 8 . . . ?
O1 Cr1 O1 C1 50.00(19) 9 . . . ?
Mn1 O2 C1 O1 -167.6(2) . . . . ?
Cr1 O1 C1 O2 -178.0(2) . . . . ?
N1 C2 N1 N1 68.0(6) 2_655 . . 3_665 ?
N1 C2 N1 N1 -68.0(6) 3_665 . . 2_655 ?
N1 C2 N1 C2 34.0(3) 2_655 . . 4_665 ?
N1 C2 N1 C2 -34.0(3) 3_665 . . 4_665 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.42
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.435
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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 1038143'
_audit_update_record             
;
2015-03-06 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H12 Cr Mn N O12'
_chemical_formula_weight         409.12

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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   8.2708(12)
_cell_length_b                   8.2708(12)
_cell_length_c                   14.088(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     834.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7695
_cell_measurement_theta_min      3.2
_cell_measurement_theta_max      27.4

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             412
_exptl_absorpt_coefficient_mu    1.461
_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      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8248
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.19
_diffrn_reflns_theta_max         27.43
_reflns_number_total             644
_reflns_number_gt                609
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL

_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)+(0.0617P)²+1.5954P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         644
_refine_ls_number_parameters     40
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_ref         0.1275
_refine_ls_wR_factor_gt          0.1252
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_restrained_S_all      1.226
_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
Mn1 Mn 0.6667 0.3333 0.2500 0.0172(3) Uani 1 6 d S . .
Cr1 Cr 0.0000 0.0000 0.0000 0.0141(3) Uani 1 6 d S . .
O2 O 0.4485(4) 0.3378(4) 0.16533(19) 0.0366(7) Uani 1 1 d . . .
O1 O 0.1902(3) 0.2040(3) 0.07992(17) 0.0254(5) Uani 1 1 d . . .
C1 C 0.3320(5) 0.2099(5) 0.1160(3) 0.0305(8) Uani 1 1 d . . .
H1A H 0.3502 0.1094 0.1046 0.037 Uiso 1 1 calc R . .
N1 N 0.2738(15) 0.548(3) 0.2500 0.068(5) Uani 0.33 2 d SPDU . .
H3B H 0.3143 0.6300 0.2988 0.082 Uiso 0.17 1 d PR . .
H3A H 0.3264 0.4685 0.2500 0.082 Uiso 0.33 1 d PR . .
C2 C 0.3333 0.6667 0.136(3) 0.15(2) Uani 0.50 3 d SPD . .
H2 H 0.3386 0.7491 0.0982 0.184 Uiso 0.50 1 d PR . .

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
Mn1 0.0156(4) 0.0156(4) 0.0204(6) 0.000 0.000 0.0078(2)
Cr1 0.0132(4) 0.0132(4) 0.0160(6) 0.000 0.000 0.0066(2)
O2 0.0312(14) 0.0333(14) 0.0462(15) -0.0146(12) -0.0204(12) 0.0167(12)
O1 0.0220(12) 0.0231(12) 0.0317(12) -0.0085(10) -0.0096(10) 0.0118(10)
C1 0.0254(16) 0.0272(17) 0.0406(19) -0.0083(15) -0.0120(15) 0.0143(14)
N1 0.049(6) 0.063(8) 0.098(9) 0.000 0.015(7) 0.032(4)
C2 0.083(13) 0.083(13) 0.30(7) 0.000 0.000 0.041(7)

_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
Mn1 O2 2.179(2) 5_655 ?
Mn1 O2 2.179(2) 2_655 ?
Mn1 O2 2.179(2) 3_665 ?
Mn1 O2 2.179(2) 6 ?
Mn1 O2 2.179(2) 4_665 ?
Mn1 O2 2.179(2) . ?
Cr1 O1 1.983(2) 7 ?
Cr1 O1 1.983(2) . ?
Cr1 O1 1.983(2) 2 ?
Cr1 O1 1.983(2) 9 ?
Cr1 O1 1.983(2) 3 ?
Cr1 O1 1.983(2) 8 ?
O2 C1 1.229(4) . ?
O1 C1 1.257(4) . ?
C1 H1A 0.9300 . ?
N1 N1 1.48(4) 2_665 ?
N1 N1 1.48(4) 3_565 ?
N1 C2 1.82(4) 4_665 ?
N1 C2 1.82(4) . ?
N1 H3B 0.9062 . ?
N1 H3A 0.9499 . ?
C2 N1 1.82(4) 3_565 ?
C2 N1 1.82(4) 2_665 ?
C2 H2 0.8474 . ?

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
O2 Mn1 O2 88.35(16) 5_655 2_655 ?
O2 Mn1 O2 85.91(14) 5_655 3_665 ?
O2 Mn1 O2 92.88(11) 2_655 3_665 ?
O2 Mn1 O2 92.88(11) 5_655 6 ?
O2 Mn1 O2 85.91(14) 2_655 6 ?
O2 Mn1 O2 178.32(14) 3_665 6 ?
O2 Mn1 O2 92.88(11) 5_655 4_665 ?
O2 Mn1 O2 178.32(14) 2_655 4_665 ?
O2 Mn1 O2 88.35(16) 3_665 4_665 ?
O2 Mn1 O2 92.88(11) 6 4_665 ?
O2 Mn1 O2 178.32(14) 5_655 . ?
O2 Mn1 O2 92.88(11) 2_655 . ?
O2 Mn1 O2 92.88(11) 3_665 . ?
O2 Mn1 O2 88.35(16) 6 . ?
O2 Mn1 O2 85.91(14) 4_665 . ?
O1 Cr1 O1 180.00(17) 7 . ?
O1 Cr1 O1 89.04(10) 7 2 ?
O1 Cr1 O1 90.96(10) . 2 ?
O1 Cr1 O1 90.96(10) 7 9 ?
O1 Cr1 O1 89.04(10) . 9 ?
O1 Cr1 O1 89.04(10) 2 9 ?
O1 Cr1 O1 89.04(10) 7 3 ?
O1 Cr1 O1 90.96(10) . 3 ?
O1 Cr1 O1 90.96(10) 2 3 ?
O1 Cr1 O1 180.00(16) 9 3 ?
O1 Cr1 O1 90.96(10) 7 8 ?
O1 Cr1 O1 89.04(10) . 8 ?
O1 Cr1 O1 180.00(14) 2 8 ?
O1 Cr1 O1 90.96(10) 9 8 ?
O1 Cr1 O1 89.04(10) 3 8 ?
C1 O2 Mn1 126.5(2) . . ?
C1 O1 Cr1 126.2(2) . . ?
O2 C1 O1 125.3(3) . . ?
O2 C1 H1A 117.4 . . ?
O1 C1 H1A 117.4 . . ?
N1 N1 N1 60.0 2_665 3_565 ?
N1 N1 C2 66.1(8) 2_665 4_665 ?
N1 N1 C2 66.1(8) 3_565 4_665 ?
N1 N1 C2 66.1(8) 2_665 . ?
N1 N1 C2 66.1(8) 3_565 . ?
C2 N1 C2 124(2) 4_665 . ?
N1 N1 H3B 55.9 2_665 . ?
N1 N1 H3B 55.5 3_565 . ?
C2 N1 H3B 12.7 4_665 . ?
C2 N1 H3B 111.4 . . ?
N1 N1 H3A 96.6 2_665 . ?
N1 N1 H3A 156.6 3_565 . ?
C2 N1 H3A 106.2 4_665 . ?
C2 N1 H3A 106.2 . . ?
H3B N1 H3A 113.2 . . ?
N1 C2 N1 47.9(17) 3_565 2_665 ?
N1 C2 N1 47.9(17) 3_565 . ?
N1 C2 N1 47.9(17) 2_665 . ?
N1 C2 H2 104.3 3_565 . ?
N1 C2 H2 122.1 2_665 . ?
N1 C2 H2 151.5 . . ?

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
O2 Mn1 O2 C1 159.7(3) 5_655 . . . ?
O2 Mn1 O2 C1 22.6(3) 2_655 . . . ?
O2 Mn1 O2 C1 115.7(3) 3_665 . . . ?
O2 Mn1 O2 C1 -63.2(3) 6 . . . ?
O2 Mn1 O2 C1 -156.2(4) 4_665 . . . ?
O1 Cr1 O1 C1 -21.8(3) 7 . . . ?
O1 Cr1 O1 C1 129.5(3) 2 . . . ?
O1 Cr1 O1 C1 -141.5(3) 9 . . . ?
O1 Cr1 O1 C1 38.5(3) 3 . . . ?
O1 Cr1 O1 C1 -50.5(3) 8 . . . ?
Mn1 O2 C1 O1 168.1(3) . . . . ?
Cr1 O1 C1 O2 179.9(3) . . . . ?
N1 N1 C2 N1 -66.3(5) 2_665 . . 3_565 ?
C2 N1 C2 N1 -33.2(2) 4_665 . . 3_565 ?
N1 N1 C2 N1 66.3(5) 3_565 . . 2_665 ?
C2 N1 C2 N1 33.2(2) 4_665 . . 2_665 ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.43
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.104
####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1038144'
_audit_update_record             
;
2015-03-06 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 Al Mn N O12'
_chemical_formula_weight         398.12

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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   8.2179(12)
_cell_length_b                   8.2179(12)
_cell_length_c                   13.646(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     798.1(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    113(2)
_cell_measurement_reflns_used    2604
_cell_measurement_theta_min      2.8622
_cell_measurement_theta_max      27.7870

_exptl_crystal_description       block
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             406
_exptl_absorpt_coefficient_mu    0.942
_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      113(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 0
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7525
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.86
_diffrn_reflns_theta_max         27.90
_reflns_number_total             639
_reflns_number_gt                597
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL


_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)+(0.0615P)²+0.8311P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         639
_refine_ls_number_parameters     40
_refine_ls_number_restraints     42
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0352
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.1018
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.226
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.005

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
Mn1 Mn 1.3333 0.6667 0.2500 0.0088(3) Uani 1 6 d SU . .
Al2 Al 1.0000 1.0000 0.0000 0.0054(3) Uani 1 6 d SU . .
O2 O 1.1107(2) 0.6617(2) 0.16447(12) 0.0207(4) Uani 1 1 d U . .
O1 O 0.98914(19) 0.8045(2) 0.07932(10) 0.0143(4) Uani 1 1 d U . .
C1 C 1.1257(3) 0.7954(3) 0.11514(15) 0.0153(4) Uani 1 1 d U . .
H1A H 1.2459 0.8957 0.1038 0.018 Uiso 1 1 calc R . .
C2 C 0.6667 0.3333 0.1618(11) 0.094(3) Uani 1 3 d SU . .
H2A H 0.7090 0.4181 0.1071 0.141 Uiso 1 1 d R . .
N1 N 0.7220(9) 0.4439(19) 0.2500 0.066(4) Uani 0.33 2 d SPU . .
H3A H 0.6679 0.5241 0.2500 0.079 Uiso 0.33 1 d PR . .

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
Mn1 0.0079(3) 0.0079(3) 0.0106(4) 0.000 0.000 0.00393(15)
Al2 0.0047(4) 0.0047(4) 0.0067(6) 0.000 0.000 0.0023(2)
O2 0.0189(8) 0.0160(8) 0.0263(8) 0.0050(6) -0.0061(6) 0.0081(6)
O1 0.0129(7) 0.0138(7) 0.0165(7) 0.0014(5) -0.0015(6) 0.0070(6)
C1 0.0143(9) 0.0154(9) 0.0172(9) 0.0027(8) -0.0001(7) 0.0082(8)
C2 0.052(3) 0.052(3) 0.178(8) 0.000 0.000 0.0259(13)
N1 0.032(4) 0.037(6) 0.131(9) 0.000 0.021(6) 0.019(3)

_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
Mn1 O2 2.1533(16) 4_775 ?
Mn1 O2 2.1533(16) . ?
Mn1 O2 2.1533(16) 6 ?
Mn1 O2 2.1533(16) 3_775 ?
Mn1 O2 2.1533(16) 2_755 ?
Mn1 O2 2.1533(16) 5_755 ?
Al2 O1 1.9022(14) 8_565 ?
Al2 O1 1.9022(14) 2_765 ?
Al2 O1 1.9022(14) 9_655 ?
Al2 O1 1.9022(14) 7_775 ?
Al2 O1 1.9022(14) . ?
Al2 O1 1.9022(14) 3_675 ?
O2 C1 1.240(3) . ?
O1 C1 1.260(2) . ?
C2 N1 1.438(14) 3_665 ?
C2 N1 1.438(14) . ?
C2 N1 1.438(14) 2_655 ?
N1 N1 1.36(2) 2_655 ?
N1 N1 1.36(2) 3_665 ?
N1 C2 1.438(14) 4_665 ?

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
O2 Mn1 O2 87.97(9) 4_775 . ?
O2 Mn1 O2 93.40(6) 4_775 6 ?
O2 Mn1 O2 85.25(9) . 6 ?
O2 Mn1 O2 85.25(9) 4_775 3_775 ?
O2 Mn1 O2 93.40(6) . 3_775 ?
O2 Mn1 O2 178.13(8) 6 3_775 ?
O2 Mn1 O2 178.13(8) 4_775 2_755 ?
O2 Mn1 O2 93.40(6) . 2_755 ?
O2 Mn1 O2 87.97(9) 6 2_755 ?
O2 Mn1 O2 93.40(6) 3_775 2_755 ?
O2 Mn1 O2 93.40(6) 4_775 5_755 ?
O2 Mn1 O2 178.13(8) . 5_755 ?
O2 Mn1 O2 93.40(6) 6 5_755 ?
O2 Mn1 O2 87.97(9) 3_775 5_755 ?
O2 Mn1 O2 85.25(9) 2_755 5_755 ?
O1 Al2 O1 180.00(7) 8_565 2_765 ?
O1 Al2 O1 90.82(6) 8_565 9_655 ?
O1 Al2 O1 89.18(6) 2_765 9_655 ?
O1 Al2 O1 90.82(6) 8_565 7_775 ?
O1 Al2 O1 89.18(6) 2_765 7_775 ?
O1 Al2 O1 90.82(6) 9_655 7_775 ?
O1 Al2 O1 89.18(6) 8_565 . ?
O1 Al2 O1 90.82(6) 2_765 . ?
O1 Al2 O1 89.18(6) 9_655 . ?
O1 Al2 O1 180.00(9) 7_775 . ?
O1 Al2 O1 89.18(6) 8_565 3_675 ?
O1 Al2 O1 90.82(6) 2_765 3_675 ?
O1 Al2 O1 180.0 9_655 3_675 ?
O1 Al2 O1 89.18(6) 7_775 3_675 ?
O1 Al2 O1 90.82(6) . 3_675 ?
C1 O2 Mn1 124.74(14) . . ?
C1 O1 Al2 127.14(13) . . ?
O2 C1 O1 124.4(2) . . ?
N1 C2 N1 56.6(10) 3_665 . ?
N1 C2 N1 56.6(10) 3_665 2_655 ?
N1 C2 N1 56.6(10) . 2_655 ?
N1 N1 N1 60.0 2_655 3_665 ?
N1 N1 C2 61.7(5) 2_655 . ?
N1 N1 C2 61.7(5) 3_665 . ?
N1 N1 C2 61.7(5) 2_655 4_665 ?
N1 N1 C2 61.7(5) 3_665 4_665 ?
C2 N1 C2 113.6(12) . 4_665 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.90
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.693
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.077
####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 1038145'

_audit_update_record             
;
2015-03-06 deposited with the CCDC.
2015-03-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H14 Cr Mg N O12'
_chemical_formula_weight         392.51

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'
Mg Mg 0.0486 0.0363 '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           trigonal
_symmetry_space_group_name_H-M   P-31c

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

_cell_length_a                   8.1565(12)
_cell_length_b                   8.1565(12)
_cell_length_c                   13.705(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     789.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7065
_cell_measurement_theta_min      27.61
_cell_measurement_theta_max      3.24

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             402
_exptl_absorpt_coefficient_mu    0.825
_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      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7875
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.24
_diffrn_reflns_theta_max         27.50
_reflns_number_total             618
_reflns_number_gt                557
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'RAPID-AUTO (Rigaku, 2004)'
_computing_cell_refinement       RAPID-AUTO
_computing_data_reduction        "CrystalStructure (Rigaku/MSC'2004)"
_computing_structure_solution    SHELXS-97
_computing_structure_refinement  SHELXL-97
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL

_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)+(0.0343P)²+2.0459P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         618
_refine_ls_number_parameters     40
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1157
_refine_ls_wR_factor_gt          0.1124
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_restrained_S_all      1.240
_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
Cr1 Cr 0.0000 0.0000 0.0000 0.0125(3) Uani 1 6 d S . .
Mg1 Mg 0.6667 0.3333 0.2500 0.0118(5) Uani 1 6 d S . .
O1 O 0.1930(3) 0.2051(3) 0.08156(16) 0.0219(5) Uani 1 1 d . . .
O2 O 0.4574(3) 0.3364(4) 0.16715(17) 0.0273(6) Uani 1 1 d . . .
C1 C 0.3354(5) 0.2069(5) 0.1172(2) 0.0262(7) Uani 1 1 d . . .
H1A H 0.3502 0.1029 0.1051 0.031 Uiso 1 1 calc R . .
C2 C 0.3333 0.6667 0.1602(19) 0.151(9) Uani 1 3 d S . .
H2B H 0.2888 0.5776 0.1072 0.181 Uiso 1 1 d R . .
N1 N 0.2802(19) 0.560(4) 0.2500 0.093(7) Uani 0.33 2 d SPU . .
H2A H 0.3343 0.4809 0.2500 0.112 Uiso 0.33 1 d PR . .

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 0.0114(4) 0.0114(4) 0.0146(5) 0.000 0.000 0.00572(19)
Mg1 0.0103(7) 0.0103(7) 0.0149(11) 0.000 0.000 0.0051(3)
O1 0.0187(11) 0.0209(12) 0.0270(11) -0.0059(9) -0.0087(9) 0.0105(9)
O2 0.0233(13) 0.0239(12) 0.0344(13) -0.0092(11) -0.0153(10) 0.0115(11)
C1 0.0242(16) 0.0244(18) 0.0335(18) -0.0072(14) -0.0075(16) 0.0148(15)
C2 0.063(5) 0.063(5) 0.33(3) 0.000 0.000 0.031(3)
N1 0.077(9) 0.081(10) 0.123(11) 0.000 0.015(8) 0.040(5)

_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 O1 1.973(2) 7 ?
Cr1 O1 1.973(2) . ?
Cr1 O1 1.973(2) 8 ?
Cr1 O1 1.973(2) 9 ?
Cr1 O1 1.973(2) 3 ?
Cr1 O1 1.973(2) 2 ?
Mg1 O2 2.060(2) 2_655 ?
Mg1 O2 2.060(2) 5_655 ?
Mg1 O2 2.060(2) 6 ?
Mg1 O2 2.060(2) 3_665 ?
Mg1 O2 2.060(2) . ?
Mg1 O2 2.060(2) 4_665 ?
O1 C1 1.253(4) . ?
O2 C1 1.234(4) . ?
C2 N1 1.44(2) 3_565 ?
C2 N1 1.44(2) 2_665 ?
C2 N1 1.44(2) . ?
N1 N1 1.30(5) 2_665 ?
N1 N1 1.30(5) 3_565 ?
N1 C2 1.44(2) 4_665 ?

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
O1 Cr1 O1 180.00(16) 7 . ?
O1 Cr1 O1 91.06(9) 7 8 ?
O1 Cr1 O1 88.94(9) . 8 ?
O1 Cr1 O1 91.06(9) 7 9 ?
O1 Cr1 O1 88.94(9) . 9 ?
O1 Cr1 O1 91.06(9) 8 9 ?
O1 Cr1 O1 88.94(9) 7 3 ?
O1 Cr1 O1 91.06(9) . 3 ?
O1 Cr1 O1 88.94(9) 8 3 ?
O1 Cr1 O1 180.00(16) 9 3 ?
O1 Cr1 O1 88.94(9) 7 2 ?
O1 Cr1 O1 91.06(9) . 2 ?
O1 Cr1 O1 180.00(13) 8 2 ?
O1 Cr1 O1 88.94(9) 9 2 ?
O1 Cr1 O1 91.06(9) 3 2 ?
O2 Mg1 O2 88.32(14) 2_655 5_655 ?
O2 Mg1 O2 86.60(14) 2_655 6 ?
O2 Mg1 O2 92.54(10) 5_655 6 ?
O2 Mg1 O2 92.54(10) 2_655 3_665 ?
O2 Mg1 O2 86.60(14) 5_655 3_665 ?
O2 Mg1 O2 178.81(14) 6 3_665 ?
O2 Mg1 O2 92.54(10) 2_655 . ?
O2 Mg1 O2 178.81(14) 5_655 . ?
O2 Mg1 O2 88.32(15) 6 . ?
O2 Mg1 O2 92.54(10) 3_665 . ?
O2 Mg1 O2 178.81(14) 2_655 4_665 ?
O2 Mg1 O2 92.54(10) 5_655 4_665 ?
O2 Mg1 O2 92.54(10) 6 4_665 ?
O2 Mg1 O2 88.32(15) 3_665 4_665 ?
O2 Mg1 O2 86.60(14) . 4_665 ?
C1 O1 Cr1 125.0(2) . . ?
C1 O2 Mg1 127.9(2) . . ?
O2 C1 O1 124.9(3) . . ?
N1 C2 N1 54(2) 3_565 2_665 ?
N1 C2 N1 54(2) 3_565 . ?
N1 C2 N1 54(2) 2_665 . ?
N1 N1 N1 60.0 2_665 3_565 ?
N1 N1 C2 63.2(11) 2_665 4_665 ?
N1 N1 C2 63.2(11) 3_565 4_665 ?
N1 N1 C2 63.2(11) 2_665 . ?
N1 N1 C2 63.2(11) 3_565 . ?
C2 N1 C2 117(3) 4_665 . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.077


#=====
