# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_bd231_a
_database_code_depnum_ccdc_archive 'CCDC 1879412'
loop_
_audit_author_name
_audit_author_address
'Bartosz Zarychta'
;Opole University
Poland
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Cr K N6, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H16 Cr K N8'
_chemical_formula_weight         339.41

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_H-M_alt        'P 4/m n c'
_space_group_name_Hall           '-P 4 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'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   8.35570(10)
_cell_length_b                   8.35570(10)
_cell_length_c                   11.8796(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     829.41(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    140
_cell_measurement_reflns_used    5809
_cell_measurement_theta_min      3.448
_cell_measurement_theta_max      29.401

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             350
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_absorpt_coefficient_mu    0.943
_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      140
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur System'
_diffrn_measurement_device       '4-circle kappa geometry goniometer'
_diffrn_measurement_method       ω--scan
_diffrn_detector_area_resol_mean 10.4508
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            5809
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.448
_diffrn_reflns_theta_max         29.401
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.960
_reflns_number_total             575
_reflns_number_gt                500
_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       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0126P)²+2.8245P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         575
_refine_ls_number_parameters     33
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.0949
_refine_ls_wR_factor_gt          0.0919
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_restrained_S_all      1.171
_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 0.5000 0.5000 1.0000 0.0140(3) Uani 1 8 d S T P . .
N1 N 0.6973(5) 0.8332(5) 1.0000 0.0539(14) Uani 1 2 d S T P . .
C1 C 0.6275(4) 0.7152(5) 1.0000 0.0217(8) Uani 1 2 d S T P . .
K1 K 0.5000 0.5000 0.5000 0.0162(3) Uani 1 8 d S T P . .
C2 C 0.5000 0.5000 0.8271(4) 0.0256(11) Uani 1 4 d S T P . .
N2 N 0.5000 0.5000 0.7293(4) 0.0495(17) Uani 1 4 d S T P . .
N1A N 0.5610(6) 0.9390(6) 0.7500 0.046(2) Uani 0.5 2 d S T P . .
H1A H 0.6062 0.8927 0.8110 0.055 Uiso 0.25 1 d R U P . .
H1B H 0.6062 0.8927 0.6890 0.055 Uiso 0.25 1 d R U P . .
C1A C 0.6016(5) 1.1016(5) 0.7500 0.0626(17) Uani 1 2 d S T P . .
H1AA H 0.7159 1.1131 0.7500 0.094 Uiso 0.5 1 d R U P . .
H1AB H 0.5578 1.1506 0.6840 0.094 Uiso 0.5 1 d R U P . .
H1AC H 0.5578 1.1506 0.8160 0.094 Uiso 0.5 1 d R U P . .

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 0.0161(4) 0.0161(4) 0.0097(5) 0.000 0.000 0.000
N1 0.0227(19) 0.0206(19) 0.118(4) 0.000 0.000 -0.0068(16)
C1 0.0171(17) 0.0192(18) 0.0287(19) 0.000 0.000 -0.0002(14)
K1 0.0190(5) 0.0190(5) 0.0106(6) 0.000 0.000 0.000
C2 0.0325(18) 0.0325(18) 0.012(2) 0.000 0.000 0.000
N2 0.070(3) 0.070(3) 0.009(3) 0.000 0.000 0.000
N1A 0.061(4) 0.061(4) 0.015(3) 0.003(3) 0.003(3) 0.046(4)
C1A 0.067(2) 0.067(2) 0.054(3) -0.011(3) 0.011(3) -0.026(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
Cr1 C2 2.054(5) 9_667 ?
Cr1 C2 2.054(5) . ?
Cr1 C1 2.090(4) 9_667 ?
Cr1 C1 2.090(4) 11_567 ?
Cr1 C1 2.090(4) 3_655 ?
Cr1 C1 2.090(4) . ?
N1 C1 1.145(6) . ?
N1 K1 2.888(4) 5_656 ?
K1 N2 2.724(5) 9_666 ?
K1 N2 2.724(5) . ?
K1 N1 2.888(4) 15_775 ?
K1 N1 2.888(4) 7_446 ?
K1 N1 2.888(4) 5_646 ?
K1 N1 2.888(4) 13_575 ?
C2 N2 1.162(7) . ?
N1A C1A 1.401(6) 2_675 ?
N1A C1A 1.401(6) . ?
N1A N1A 1.442(13) 2_675 ?
N1A H1A 0.9039 . ?
N1A H1B 0.9039 . ?
C1A N1A 1.401(6) 2_675 ?
C1A H1AA 0.9593 . ?
C1A H1AB 0.9571 . ?
C1A H1AC 0.9571 . ?

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
C2 Cr1 C2 180.0 9_667 . ?
C2 Cr1 C1 90.000(1) 9_667 9_667 ?
C2 Cr1 C1 90.000(1) . 9_667 ?
C2 Cr1 C1 90.000(1) 9_667 11_567 ?
C2 Cr1 C1 90.000(1) . 11_567 ?
C1 Cr1 C1 90.0 9_667 11_567 ?
C2 Cr1 C1 90.000(1) 9_667 3_655 ?
C2 Cr1 C1 90.000(1) . 3_655 ?
C1 Cr1 C1 90.000(1) 9_667 3_655 ?
C1 Cr1 C1 180.0 11_567 3_655 ?
C2 Cr1 C1 90.000(1) 9_667 . ?
C2 Cr1 C1 90.000(1) . . ?
C1 Cr1 C1 180.0 9_667 . ?
C1 Cr1 C1 90.000(1) 11_567 . ?
C1 Cr1 C1 90.000(1) 3_655 . ?
C1 N1 K1 149.5(3) . 5_656 ?
N1 C1 Cr1 180.0(3) . . ?
N2 K1 N2 180.0 9_666 . ?
N2 K1 N1 90.000(1) 9_666 15_775 ?
N2 K1 N1 90.000(1) . 15_775 ?
N2 K1 N1 90.000(1) 9_666 7_446 ?
N2 K1 N1 90.000(1) . 7_446 ?
N1 K1 N1 180.0 15_775 7_446 ?
N2 K1 N1 90.0 9_666 5_646 ?
N2 K1 N1 90.0 . 5_646 ?
N1 K1 N1 90.0 15_775 5_646 ?
N1 K1 N1 90.0 7_446 5_646 ?
N2 K1 N1 90.0 9_666 13_575 ?
N2 K1 N1 90.0 . 13_575 ?
N1 K1 N1 90.0 15_775 13_575 ?
N1 K1 N1 90.000(1) 7_446 13_575 ?
N1 K1 N1 180.0 5_646 13_575 ?
N2 C2 Cr1 180.0 . . ?
C2 N2 K1 180.0 . . ?
C1A N1A C1A 118.0(5) 2_675 . ?
C1A N1A N1A 59.0(3) 2_675 2_675 ?
C1A N1A N1A 59.0(3) . 2_675 ?
C1A N1A H1A 107.5 2_675 . ?
C1A N1A H1A 108.3 . . ?
N1A N1A H1A 126.7 2_675 . ?
C1A N1A H1B 107.5 2_675 . ?
C1A N1A H1B 108.3 . . ?
N1A N1A H1B 126.7 2_675 . ?
H1A N1A H1B 106.6 . . ?
N1A C1A N1A 62.0(5) . 2_675 ?
N1A C1A H1AA 109.7 . . ?
N1A C1A H1AA 171.7 2_675 . ?
N1A C1A H1AB 108.8 . . ?
N1A C1A H1AB 74.5 2_675 . ?
H1AA C1A H1AB 109.8 . . ?
N1A C1A H1AC 108.8 . . ?
N1A C1A H1AC 74.5 2_675 . ?
H1AA C1A H1AC 109.8 . . ?
H1AB C1A H1AC 110.0 . . ?

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
C1A N1A C1A N1A 0.0 2_675 . . 2_675 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1A H1A N1 0.90 2.42 3.301(3) 164.2 .
N1A H1B N1 0.90 2.42 3.301(3) 164.5 15_775
C1A H1AA N2 0.96 2.57 3.444(3) 152.1 5_656

_refine_diff_density_max         0.461
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.079

_shelxl_version_number           2014-3

_shelx_res_file                  
;
TITL bd231_a.res in P4/mnc
REM Old TITL BD231 in P4/mnc
REM SHELXT solution in P4/mnc
REM R1 0.143,  Rweak 0.075,  Alpha 0.127,  Orientation as input
REM Formula found by SHELXT:  C7 N3 Cr
CELL  0.71073   8.3557   8.3557  11.8796   90.000   90.000   90.000
ZERR    2.000   0.0001   0.0001   0.0003    0.000    0.000    0.000
LATT  1
SYMM -X, -Y, Z
SYMM -Y, X, Z
SYMM Y, -X, Z
SYMM 1/2-X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SYMM 1/2+Y, 1/2+X, 1/2-Z
SYMM 1/2-Y, 1/2-X, 1/2-Z
SFAC C H N K CR
UNIT 20 32 16 2 2
ACTA

OMIT    1   4   3
OMIT     0   3   1
OMIT     0   1   9
OMIT     1   3   3
OMIT     0   1   1
OMIT     0   1   5
OMIT     1   4   1
OMIT     1   3   7
OMIT     0   3   3
OMIT     0   1  13
OMIT     1   2   3
OMIT     0   0   2
OMIT     4   5   5
OMIT     0   5   3
OMIT     1   3   1
OMIT     1   2   5
HTAB N1A N1
EQIV $1 -y+3/2, -x+3/2, z-1/2
HTAB N1A N1_$1
EQIV $2 -x+3/2, y+1/2, -z+3/2
HTAB C1A N2_$2
CONF
L.S. 10
BOND $H
LIST 6
FMAP 2
PLAN 20
WGHT    0.012600    2.824500
FVAR       0.52308
CR1   5    0.500000    0.500000    1.000000    10.12500    0.01614    0.01614 =
         0.00968    0.00000    0.00000    0.00000
N1    3    0.697324    0.833182    1.000000    10.50000    0.02270    0.02055 =
         0.11836    0.00000    0.00000   -0.00680
C1    1    0.627538    0.715222    1.000000    10.50000    0.01714    0.01920 =
         0.02869    0.00000    0.00000   -0.00023
K1    4    0.500000    0.500000    0.500000    10.12500    0.01897    0.01897 =
         0.01061    0.00000    0.00000    0.00000
C2    1    0.500000    0.500000    0.827106    10.25000    0.03247    0.03247 =
         0.01175    0.00000    0.00000    0.00000
N2    3    0.500000    0.500000    0.729317    10.25000    0.06960    0.06960 =
         0.00937    0.00000    0.00000    0.00000

N1A   3    0.561029    0.938971    0.750000    10.25000    0.06129    0.06129 =
         0.01536    0.00330    0.00330    0.04623
AFIX   3
H1A   2    0.606169    0.892720    0.811020    10.25000   -1.20000
H1B   2    0.606169    0.892720    0.688980    10.25000   -1.20000
AFIX   0
C1A   1    0.601632    1.101632    0.750000    10.50000    0.06702    0.06702 =
         0.05382   -0.01098    0.01098   -0.02610
AFIX   3
H1AA  2    0.715870    1.113080    0.750000    10.50000   -1.50000
H1AB  2    0.557782    1.150610    0.684020    10.50000   -1.50000
H1AC  2    0.557782    1.150610    0.815980    10.50000   -1.50000

REM #####
AFIX   0
HKLF 4

REM  bd231_a.res in P4/mnc
REM R1 =  0.0470 for     500 Fo > 4sig(Fo)  and  0.0550 for all     575 data
REM     33 parameters refined using      0 restraints

END

WGHT      0.0129      2.8224

REM Highest difference peak  0.461,  deepest hole -0.392,  1-sigma level  0.079
Q1    1   0.6753  0.8040  1.0412  11.00000  0.05    0.46
Q2    1   0.5000  0.5000  0.3952  10.25000  0.05    0.42
Q3    1   0.6021  0.7498  1.0000  10.50000  0.05    0.33
Q4    1   0.6561  0.8976  1.0000  10.50000  0.05    0.31
Q5    1   0.3832  0.6321  0.5000  10.50000  0.05    0.28
Q6    1   0.4432  0.8367  1.0000  10.50000  0.05    0.28
Q7    1   0.6736  1.0794  0.7331  11.00000  0.05    0.27
Q8    1   0.6008  0.6699  1.0307  11.00000  0.05    0.23
Q9    1   0.4244  0.4500  0.6987  11.00000  0.05    0.22
Q10   1   0.8755  0.7284  1.0000  10.50000  0.05    0.22
Q11   1   0.4796  0.4563  0.7446  11.00000  0.05    0.22
Q12   1   0.5178  0.6531  1.0000  10.50000  0.05    0.22
Q13   1   0.6957  1.1957  0.7500  10.50000  0.05    0.21
Q14   1   0.6969  0.6275  1.0578  11.00000  0.05    0.21
Q15   1   0.5584  0.5997  0.4492  11.00000  0.05    0.19
Q16   1   0.8023  1.0302  0.7672  11.00000  0.05    0.19
Q17   1   0.6036  0.5824  0.5000  10.50000  0.05    0.19
Q18   1   0.5673  0.4504  0.7384  11.00000  0.05    0.19
Q19   1   0.8529  0.8818  1.1144  11.00000  0.05    0.17
Q20   1   0.4932  0.4275  0.7820  11.00000  0.05    0.17
;
_shelx_res_checksum              47095
####################################################################### 
# 
# 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_bd230_a
_database_code_depnum_ccdc_archive 'CCDC 1879413'
loop_
_audit_author_name
_audit_author_address
'Bartosz Zarychta'
;Opole University
Poland
;
_audit_update_record             
;
2018-11-16 deposited with the CCDC.	2019-02-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C6 Cr K N6, 2(C2 H8 N)'
_chemical_formula_sum            'C10 H16 Cr K N8'
_chemical_formula_weight         339.41

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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      tetragonal
_space_group_IT_number           128
_space_group_name_H-M_alt        'P 4/m n c'
_space_group_name_Hall           '-P 4 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'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   8.40300(10)
_cell_length_b                   8.40300(10)
_cell_length_c                   11.8999(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     840.26(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    230
_cell_measurement_reflns_used    6061
_cell_measurement_theta_min      3.424
_cell_measurement_theta_max      29.508

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_F_000             350
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_exptl_absorpt_coefficient_mu    0.931
_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      230
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur System'
_diffrn_measurement_device       '4-circle kappa geometry goniometer'
_diffrn_measurement_method       ω--scan
_diffrn_detector_area_resol_mean 10.4508
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            6061
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_av_R_equivalents  0.0205
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.424
_diffrn_reflns_theta_max         29.508
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             597
_reflns_number_gt                446
_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       'CrysAlis CCD (Oxford Diffraction, 2007)'
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2007)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²+0.0902P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0096(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         597
_refine_ls_number_parameters     39
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0603
_refine_ls_wR_factor_gt          0.0563
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_restrained_S_all      1.213
_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 0.5000 0.5000 0.0000 0.02301(17) Uani 1 8 d S T P . .
K1 K 0.5000 0.5000 0.5000 0.02818(18) Uani 1 8 d S T P . .
C1 C 0.2893(2) 0.3699(2) 0.0000 0.0364(4) Uani 1 2 d S T P . .
N1 N 0.1733(2) 0.2998(2) 0.0000 0.0687(6) Uani 1 2 d S T P . .
C2 C 0.5000 0.5000 0.1731(2) 0.0444(7) Uani 1 4 d S T P . .
N2 N 0.5000 0.5000 0.2690(2) 0.0858(13) Uani 1 4 d S T P . .
C1A C 0.4002(3) 0.0998(3) 0.2500 0.1010(11) Uani 1 2 d S TU P A 1
H1AC H 0.2866 0.1125 0.2500 0.151 Uiso 0.5 1 d R U P A 1
H1AD H 0.4437 0.1504 0.3159 0.151 Uiso 0.5 1 d R U P A 1
H1AE H 0.4437 0.1504 0.1841 0.151 Uiso 0.5 1 d R U P A 1
N1AA N 0.4377(6) -0.0623(6) 0.2500 0.0558(15) Uani 0.3 2 d S TU P A 1
H1AA H 0.3928 -0.1065 0.1891 0.067 Uiso 0.15 1 d R U P A 1
H1AB H 0.3928 -0.1065 0.3109 0.067 Uiso 0.15 1 d R U P A 1
N1AB N 0.5000 0.0000 0.1851(12) 0.095(4) Uani 0.2 2 d S TU P B 2
H1AF H 0.5610 0.0611 0.1403 0.114 Uiso 0.1 1 d R U P B 2
H1AG H 0.4390 -0.0611 0.1403 0.114 Uiso 0.1 1 d R U P B 2

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 0.02659(19) 0.02659(19) 0.0159(2) 0.000 0.000 0.000
K1 0.0332(2) 0.0332(2) 0.0181(3) 0.000 0.000 0.000
C1 0.0369(9) 0.0339(9) 0.0383(9) 0.000 0.000 -0.0014(7)
N1 0.0454(10) 0.0528(11) 0.1081(18) 0.000 0.000 -0.0147(10)
C2 0.0551(10) 0.0551(10) 0.0228(12) 0.000 0.000 0.000
N2 0.117(2) 0.117(2) 0.0238(14) 0.000 0.000 0.000
C1A 0.0959(15) 0.0959(15) 0.111(3) 0.0173(13) 0.0173(13) 0.026(2)
N1AA 0.066(2) 0.066(2) 0.035(3) 0.0005(18) -0.0005(18) -0.027(3)
N1AB 0.117(8) 0.125(9) 0.043(6) 0.000 0.000 -0.073(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
Cr1 C2 2.060(3) 9_665 ?
Cr1 C2 2.060(3) . ?
Cr1 C1 2.0805(17) 9_665 ?
Cr1 C1 2.0805(17) 11_565 ?
Cr1 C1 2.0805(17) 3_655 ?
Cr1 C1 2.0806(17) . ?
K1 N2 2.749(3) 9_666 ?
K1 N2 2.749(3) . ?
K1 N1 2.9100(17) 15_666 ?
K1 N1 2.9100(17) 7 ?
K1 N1 2.9100(16) 5 ?
K1 N1 2.9100(16) 13_666 ?
C1 N1 1.139(2) . ?
N1 K1 2.9100(16) 5_545 ?
C2 N2 1.141(3) . ?
C1A N1AA 1.398(5) 2_655 ?
C1A N1AA 1.398(5) . ?
C1A H1AC 0.9609 . ?
C1A H1AD 0.9637 . ?
C1A H1AE 0.9637 . ?
N1AA C1A 1.398(5) 2_655 ?
N1AA N1AA 1.481(14) 2_655 ?
N1AA H1AA 0.8975 . ?
N1AA H1AB 0.8975 . ?
N1AB N1AB 1.55(3) 7_545 ?
N1AB H1AF 0.9000 . ?
N1AB H1AG 0.9000 . ?

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
C2 Cr1 C2 180.0 9_665 . ?
C2 Cr1 C1 90.0 9_665 9_665 ?
C2 Cr1 C1 90.0 . 9_665 ?
C2 Cr1 C1 90.0 9_665 11_565 ?
C2 Cr1 C1 90.0 . 11_565 ?
C1 Cr1 C1 90.0 9_665 11_565 ?
C2 Cr1 C1 90.0 9_665 3_655 ?
C2 Cr1 C1 90.0 . 3_655 ?
C1 Cr1 C1 90.0 9_665 3_655 ?
C1 Cr1 C1 180.0 11_565 3_655 ?
C2 Cr1 C1 90.0 9_665 . ?
C2 Cr1 C1 90.0 . . ?
C1 Cr1 C1 180.0 9_665 . ?
C1 Cr1 C1 90.0 11_565 . ?
C1 Cr1 C1 90.0 3_655 . ?
N2 K1 N2 180.0 9_666 . ?
N2 K1 N1 90.0 9_666 15_666 ?
N2 K1 N1 90.0 . 15_666 ?
N2 K1 N1 90.0 9_666 7 ?
N2 K1 N1 90.0 . 7 ?
N1 K1 N1 180.00(6) 15_666 7 ?
N2 K1 N1 90.0 9_666 5 ?
N2 K1 N1 90.0 . 5 ?
N1 K1 N1 90.0 15_666 5 ?
N1 K1 N1 90.0 7 5 ?
N2 K1 N1 90.0 9_666 13_666 ?
N2 K1 N1 90.0 . 13_666 ?
N1 K1 N1 90.0 15_666 13_666 ?
N1 K1 N1 90.0 7 13_666 ?
N1 K1 N1 180.0 5 13_666 ?
N1 C1 Cr1 179.45(17) . . ?
C1 N1 K1 151.16(16) . 5_545 ?
N2 C2 Cr1 180.0 . . ?
C2 N2 K1 180.0 . . ?
N1AA C1A N1AA 64.0(5) 2_655 . ?
N1AA C1A H1AC 173.4 2_655 . ?
N1AA C1A H1AC 109.4 . . ?
N1AA C1A H1AD 74.4 2_655 . ?
N1AA C1A H1AD 110.2 . . ?
H1AC C1A H1AD 109.1 . . ?
N1AA C1A H1AE 74.4 2_655 . ?
N1AA C1A H1AE 110.2 . . ?
H1AC C1A H1AE 109.1 . . ?
H1AD C1A H1AE 108.9 . . ?
C1A N1AA C1A 116.0(5) 2_655 . ?
C1A N1AA N1AA 58.0(3) 2_655 2_655 ?
C1A N1AA N1AA 58.0(3) . 2_655 ?
C1A N1AA H1AA 108.4 2_655 . ?
C1A N1AA H1AA 108.0 . . ?
N1AA N1AA H1AA 126.2 2_655 . ?
C1A N1AA H1AB 108.4 2_655 . ?
C1A N1AA H1AB 108.0 . . ?
N1AA N1AA H1AB 126.2 2_655 . ?
H1AA N1AA H1AB 107.7 . . ?
N1AB N1AB H1AF 126.3 7_545 . ?
N1AB N1AB H1AG 126.3 7_545 . ?
H1AF N1AB H1AG 107.4 . . ?

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
N1AA C1A N1AA C1A 0.0 2_655 . . 2_655 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C1A H1AC N2 0.96 2.60 3.4735(19) 151.7 5_545
N1AA H1AA N1 0.90 2.45 3.326(3) 166.3 11
N1AA H1AB N1 0.90 2.45 3.326(3) 166.1 5_545

_refine_diff_density_max         0.225
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.036

_shelxl_version_number           2013-4

_shelx_res_file                  
;
TITL bd230_a.res in P4/mnc
REM Old TITL bd230 in P4/mnc

REM SHELXT solution in P4/mnc
REM R1 0.124,  Rweak 0.002,  Alpha 0.021,  Orientation as input
REM Formula found by SHELXT:  C10 N6 K Cr

CELL  0.71073   8.4030   8.4030  11.8999   90.000   90.000   90.000
ZERR    2.000   0.0001   0.0001   0.0003    0.000    0.000    0.000
LATT  1
SYMM -X, -Y, Z
SYMM -Y, X, Z
SYMM Y, -X, Z
SYMM 1/2-X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SYMM 1/2+Y, 1/2+X, 1/2-Z
SYMM 1/2-Y, 1/2-X, 1/2-Z
SFAC C H N K CR
UNIT 20 32 16 2 2
ACTA
L.S. 10
EQIV $1 -x+1/2, y-1/2, -z+1/2
HTAB C1A N2_$1
EQIV $2 y, -x, -z
HTAB N1AA N1_$2
HTAB N1AA N1_$1
EQIV $3 -y+1, x, z

CONF
OMIT     6   8   8
OMIT     0   1   1
OMIT     0   3   1
OMIT     1   2   3
OMIT     0   2   2
OMIT     0   3   5
OMIT     2   3   3
BOND $H
LIST 6
FMAP 2
SIMU 0.01 C1a > N1ab
DELU 0.01 C1a > N1ab
PLAN 20
WGHT    0.031200    0.090200
EXTI    0.009628
FVAR       0.62212
CR1   5    0.500000    0.500000    0.000000    10.12500    0.02659    0.02659 =
         0.01586    0.00000    0.00000    0.00000
K1    4    0.500000    0.500000    0.500000    10.12500    0.03322    0.03322 =
         0.01809    0.00000    0.00000    0.00000
C1    1    0.289311    0.369945    0.000000    10.50000    0.03693    0.03390 =
         0.03834    0.00000    0.00000   -0.00139
N1    3    0.173275    0.299844    0.000000    10.50000    0.04538    0.05280 =
         0.10805    0.00000    0.00000   -0.01471
C2    1    0.500000    0.500000    0.173149    10.25000    0.05514    0.05514 =
         0.02281    0.00000    0.00000    0.00000
N2    3    0.500000    0.500000    0.269024    10.25000    0.11684    0.11684 =
         0.02375    0.00000    0.00000    0.00000

part 1
C1A   1    0.400236    0.099764    0.250000    10.50000    0.09587    0.09587 =
         0.11113    0.01733    0.01733    0.02566
AFIX   3
H1AC  2    0.286595    0.112520    0.250000    10.50000   -1.50000
H1AD  2    0.443655    0.150420    0.315870    10.50000   -1.50000
H1AE  2    0.443655    0.150420    0.184130    10.50000   -1.50000
AFIX   0
N1AA  3    0.437704   -0.062296    0.250000    10.15000    0.06645    0.06645 =
         0.03450    0.00053   -0.00053   -0.02665
AFIX   3
H1AA  2    0.392794   -0.106500    0.189100    10.15000   -1.20000
H1AB  2    0.392794   -0.106500    0.310900    10.15000   -1.20000
AFIX   0
Part 2
N1AB  3    0.500000    0.000000    0.185076    10.10000    0.11687    0.12494 =
         0.04322    0.00000    0.00000   -0.07279
AFIX   3
H1AF  2    0.561050    0.061050    0.140316    10.10000   -1.20000
H1AG  2    0.438950   -0.061050    0.140316    10.10000   -1.20000
part 0
REM #####
REM #####
AFIX   0
HKLF 4

REM  bd230_a.res in P4/mnc
REM R1 =  0.0219 for     446 Fo > 4sig(Fo)  and  0.0349 for all     597 data
REM     39 parameters refined using     19 restraints

END

WGHT      0.0312      0.0902

REM Highest difference peak  0.225,  deepest hole -0.299,  1-sigma level  0.036
Q1    1   0.5000  0.5000  0.0998  10.25000  0.05    0.22
Q2    1   0.2136  0.3018 -0.0451  11.00000  0.05    0.16
Q3    1   0.3728  0.4206  0.0000  10.50000  0.05    0.14
Q4    1   0.4337  0.0453  0.1882  11.00000  0.05    0.14
Q5    1   0.2151  0.2292  0.0000  10.50000  0.05    0.12
Q6    1   0.4762  0.0856  0.1874  11.00000  0.05    0.11
Q7    1   0.3034  0.3160  0.0000  10.50000  0.05    0.11
Q8    1   0.4325  0.5788  0.5000  10.50000  0.05    0.11
Q9    1   0.4913  0.1473  0.1843  11.00000  0.05    0.11
Q10   1   0.4873  0.5467  0.3588  11.00000  0.05    0.10
Q11   1   0.2923  0.2077  0.2500  10.50000  0.05    0.10
Q12   1   0.5000  0.5000  0.3865  10.25000  0.05    0.09
Q13   1   0.2332  0.4007  0.0000  10.50000  0.05    0.09
Q14   1   0.4847  0.6027  0.2755  11.00000  0.05    0.08
Q15   1   0.4223  0.4998  0.2278  11.00000  0.05    0.08
Q16   1   0.5207  0.2019  0.2788  11.00000  0.05    0.07
Q17   1   0.2506 -0.1843  0.1827  11.00000  0.05    0.07
Q18   1   0.0394  0.3765  0.0000  10.50000  0.05    0.07
Q19   1   0.4544  0.6707  0.4492  11.00000  0.05    0.07
Q20   1   0.1735  0.1379 -0.0433  11.00000  0.05    0.06
;
_shelx_res_checksum              35577
