# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
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data_RDB-1-CrStBu
_audit_creation_date             2014-04-02
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2900 for OlexSys, GUI svn.r4781)
;
_chemical_formula_moiety         'C16 H37 Cr N3 S'
_chemical_formula_sum            'C16 H37 Cr N3 S'
_chemical_formula_weight         355.55
_chemical_absolute_configuration unk
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cr 0.32644 0.61635 10.64060 7.35370 3.32400 1.49220 6.10380 0.39200 20.26260
98.73990 1.18320000172
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
S 0.12424 0.12443 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360
56.17200 0.866900026798
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 x+1/2,-y+1/2,-z
3 -x,y+1/2,-z+1/2
4 -x+1/2,-y,z+1/2

_symmetry_Int_Tables_number      19
_cell_length_a                   9.9625(8)
_cell_length_b                   10.7349(9)
_cell_length_c                   19.7412(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2111.3(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      25.365
_cell_measurement_theta_min      2.290
_exptl_absorpt_coefficient_mu    0.640
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1375 before and 0.0525 after correction.
The Ratio of minimum to maximum transmission is 0.9019.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.1185
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             777.9602
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.193
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17438
_diffrn_reflns_theta_full        25.3738
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         2.06
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9984
_diffrn_measured_fraction_theta_max 0.9984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.998
_reflns_limit_h_max              12
_reflns_limit_h_min              -11
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              23
_reflns_limit_l_min              -23
_reflns_number_gt                3613
_reflns_number_total             3861
_reflns_threshold_expression     I>=2u(I)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_data_collection       cosmo
_computing_structure_solution    shelxT
_refine_diff_density_max         0.5131
_refine_diff_density_min         -0.2985
_refine_diff_density_rms         0.0497
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   -0.06(2)
_refine_ls_d_res_high            0.8293
_refine_ls_d_res_low             9.8706
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     201
_refine_ls_number_reflns         3861
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0334
_refine_ls_restrained_S_all      1.0329
_refine_ls_shift/su_max          0.0177
_refine_ls_shift/su_mean         0.0018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0483P)²+0.7135P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0887
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C22(H22), C31(H31), C21(H21), C32(H32)
2.b Idealised Me refined as rotating group:
 C222(H22a,H22b,H22c), C312(H31a,H31b,H31c), C311(H31d,H31e,H31f), C221(H22d,
 H22e,H22f), C212(H21a,H21b,H21c), C211(H21d,H21e,H21f), C321(H32a,H32b,H32c),
 C322(H32d,H32e,H32f), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C2(H2a,H2b,H2c)
;
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_refinement_flags_posn
Cr1 Cr 0.8042504(17) 0.0859946(17) 0.8632656(17) 0.02647(8) Uani 1.000000 .
C222 C 0.7396784(17) 0.0183997(17) 0.6766861(17) 0.0523(2) Uani 1.000000 .
H22a H 0.6881713(17) -0.0426662(17) 0.7028784(17) 0.0784(3) Uiso 1.000000 GR
H22b H 0.6781054(17) 0.0784295(17) 0.6558714(17) 0.0784(3) Uiso 1.000000 GR
H22c H 0.7905557(17) -0.0245501(17) 0.6411943(17) 0.0784(3) Uiso 1.000000 GR
C22 C 0.8362373(17) 0.0866799(17) 0.7234330(17) 0.0397(2) Uani 1.000000 .
H22 H 0.8959761(17) 0.0220779(17) 0.7440007(17) 0.0477(3) Uiso 1.000000 R
N2 N 0.7632183(17) 0.1466630(17) 0.7799225(17) 0.0294(2) Uani 1.000000 .
N3 N 0.9645118(17) 0.1294415(17) 0.9002398(17) 0.0313(2) Uani 1.000000 .
C31 C 1.0830117(17) 0.0811969(17) 0.8632452(17) 0.0451(2) Uani 1.000000 .
H31 H 1.0478329(17) 0.0331489(17) 0.8236453(17) 0.0541(3) Uiso 1.000000 R
C312 C 1.1602027(17) -0.0105570(17) 0.9068607(17) 0.0624(2) Uani 1.000000 .
H31a H 1.1996084(17) 0.0333488(17) 0.9455761(17) 0.0936(3) Uiso 1.000000 GR
H31b H 1.0990552(17) -0.0754124(17) 0.9232422(17) 0.0936(3) Uiso 1.000000 GR
H31c H 1.2317931(17) -0.0488608(17) 0.8799302(17) 0.0936(3) Uiso 1.000000 GR
C311 C 1.1710401(17) 0.1825526(17) 0.8348985(17) 0.0656(2) Uani 1.000000 .
H31d H 1.1155980(17) 0.2428015(17) 0.8102374(17) 0.0984(3) Uiso 1.000000 GR
H31e H 1.2177265(17) 0.2248653(17) 0.8720450(17) 0.0984(3) Uiso 1.000000 GR
H31f H 1.2371032(17) 0.1459747(17) 0.8039592(17) 0.0984(3) Uiso 1.000000 GR
C221 C 0.9258924(17) 0.1746221(17) 0.6844175(17) 0.0580(2) Uani 1.000000 .
H22d H 0.9756191(17) 0.1279114(17) 0.6499294(17) 0.0870(3) Uiso 1.000000 GR
H22e H 0.8709011(17) 0.2385997(17) 0.6624203(17) 0.0870(3) Uiso 1.000000 GR
H22f H 0.9893164(17) 0.2144034(17) 0.7155935(17) 0.0870(3) Uiso 1.000000 GR
C21 C 0.6671927(17) 0.2439306(17) 0.7601064(17) 0.0416(2) Uani 1.000000 .
H21 H 0.6724575(17) 0.2534063(17) 0.7097837(17) 0.0499(3) Uiso 1.000000 R
C212 C 0.5238106(17) 0.2055935(17) 0.7777115(17) 0.0556(2) Uani 1.000000 .
H21a H 0.5077238(17) 0.1202458(17) 0.7620742(17) 0.0834(3) Uiso 1.000000 GR
H21b H 0.5111983(17) 0.2097168(17) 0.8268930(17) 0.0834(3) Uiso 1.000000 GR
H21c H 0.4604677(17) 0.2622079(17) 0.7554685(17) 0.0834(3) Uiso 1.000000 GR
C211 C 0.7040077(17) 0.3680569(17) 0.7913554(17) 0.0668(2) Uani 1.000000 .
H21d H 0.6937903(17) 0.3632533(17) 0.8406601(17) 0.1003(3) Uiso 1.000000 GR
H21e H 0.7973552(17) 0.3882696(17) 0.7802035(17) 0.1003(3) Uiso 1.000000 GR
H21f H 0.6447161(17) 0.4330218(17) 0.7734370(17) 0.1003(3) Uiso 1.000000 GR
N1 N 0.6990284(17) 0.1424680(17) 0.9120763(17) 0.0355(2) Uani 1.000000 .
C32 C 0.9947093(17) 0.2078168(17) 0.9593507(17) 0.0460(2) Uani 1.000000 .
H32 H 1.0945385(17) 0.2123103(17) 0.9640335(17) 0.0552(3) Uiso 1.000000 R
C321 C 0.9430291(17) 0.3394210(17) 0.9495716(17) 0.0583(2) Uani 1.000000 .
H32a H 0.9710445(17) 0.3703646(17) 0.9050593(17) 0.0875(3) Uiso 1.000000 GR
H32b H 0.8448098(17) 0.3395432(17) 0.9523077(17) 0.0875(3) Uiso 1.000000 GR
H32c H 0.9798248(17) 0.3934294(17) 0.9850261(17) 0.0875(3) Uiso 1.000000 GR
C322 C 0.9387451(17) 0.1504806(17) 1.0243522(17) 0.0590(2) Uani 1.000000 .
H32d H 0.8404353(17) 0.1525303(17) 1.0230412(17) 0.0886(3) Uiso 1.000000 GR
H32e H 0.9692594(17) 0.0639807(17) 1.0281921(17) 0.0886(3) Uiso 1.000000 GR
H32f H 0.9706591(17) 0.1981696(17) 1.0634992(17) 0.0886(3) Uiso 1.000000 GR
C3 C 0.6981595(17) -0.1501639(17) 0.9938479(17) 0.0863(2) Uani 1.000000 .
H3a H 0.6333545(17) -0.1872410(17) 1.0252851(17) 0.1294(3) Uiso 1.000000 GR
H3b H 0.7878621(17) -0.1834468(17) 1.0032038(17) 0.1294(3) Uiso 1.000000 GR
H3c H 0.6988585(17) -0.0595116(17) 0.9996995(17) 0.1294(3) Uiso 1.000000 GR
C1 C 0.6586568(17) -0.1814804(17) 0.9218619(17) 0.0402(2) Uani 1.000000 .
C4 C 0.6581872(17) -0.3230831(17) 0.9103773(17) 0.0697(2) Uani 1.000000 .
H4a H 0.7456065(17) -0.3576258(17) 0.9232326(17) 0.1046(3) Uiso 1.000000 GR
H4b H 0.5877535(17) -0.3612598(17) 0.9381256(17) 0.1046(3) Uiso 1.000000 GR
H4c H 0.6409021(17) -0.3406555(17) 0.8624506(17) 0.1046(3) Uiso 1.000000 GR
C2 C 0.5214489(17) -0.1276302(17) 0.9058967(17) 0.0757(2) Uani 1.000000 .
H2a H 0.4543771(17) -0.1646458(17) 0.9361211(17) 0.1135(4) Uiso 1.000000 GR
H2b H 0.5232592(17) -0.0371665(17) 0.9125018(17) 0.1135(4) Uiso 1.000000 GR
H2c H 0.4980862(17) -0.1462959(17) 0.8587550(17) 0.1135(4) Uiso 1.000000 GR
S1 S 0.7811311(17) -0.1219552(17) 0.8616010(17) 0.05363(14) Uani 1.000000 .


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 N2 1.81611(13) . ?
Cr1 N3 1.81644(12) . ?
Cr1 N1 1.54754(9) . ?
Cr1 S1 2.24441(19) . ?
C222 H22a 0.9800 . ?
C222 H22b 0.9800 . ?
C222 H22c 0.9800 . ?
C222 C22 1.52127(8) . ?
C22 H22 1.0000 . ?
C22 N2 1.47899(9) . ?
C22 C221 1.51071(8) . ?
N2 C21 1.46918(8) . ?
N3 C31 1.48165(9) . ?
N3 C32 1.46972(10) . ?
C31 H31 1.0000 . ?
C31 C312 1.51753(8) . ?
C31 C311 1.50535(8) . ?
C312 H31a 0.9800 . ?
C312 H31b 0.9800 . ?
C312 H31c 0.9800 . ?
C311 H31d 0.9800 . ?
C311 H31e 0.9800 . ?
C311 H31f 0.9800 . ?
C221 H22d 0.9800 . ?
C221 H22e 0.9800 . ?
C221 H22f 0.9800 . ?
C21 H21 1.0000 . ?
C21 C212 1.52663(11) . ?
C21 C211 1.51347(11) . ?
C212 H21a 0.9800 . ?
C212 H21b 0.9800 . ?
C212 H21c 0.9800 . ?
C211 H21d 0.9800 . ?
C211 H21e 0.9800 . ?
C211 H21f 0.9800 . ?
C32 H32 1.0000 . ?
C32 C321 1.51599(11) . ?
C32 C322 1.52850(10) . ?
C321 H32a 0.9800 . ?
C321 H32b 0.9800 . ?
C321 H32c 0.9800 . ?
C322 H32d 0.9800 . ?
C322 H32e 0.9800 . ?
C322 H32f 0.9800 . ?
C3 H3a 0.9800 . ?
C3 H3b 0.9800 . ?
C3 H3c 0.9800 . ?
C3 C1 1.51241(12) . ?
C1 C4 1.53691(13) . ?
C1 C2 1.51724(10) . ?
C1 S1 1.81997(10) . ?
C4 H4a 0.9800 . ?
C4 H4b 0.9800 . ?
C4 H4c 0.9800 . ?
C2 H2a 0.9800 . ?
C2 H2b 0.9800 . ?
C2 H2c 0.9800 . ?

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
N3 Cr1 N2 118.0221(17) . . ?
N1 Cr1 N2 105.7320(17) . . ?
N1 Cr1 N3 104.159(2) . . ?
S1 Cr1 N2 108.6818(17) . . ?
S1 Cr1 N3 110.5771(13) . . ?
S1 Cr1 N1 109.2222(15) . . ?
H22b C222 H22a 109.5 . . ?
H22c C222 H22a 109.5 . . ?
H22c C222 H22b 109.5 . . ?
C22 C222 H22a 109.5 . . ?
C22 C222 H22b 109.5 . . ?
C22 C222 H22c 109.5 . . ?
H22 C22 C222 106.7685(11) . . ?
N2 C22 C222 110.8638(17) . . ?
N2 C22 H22 106.7685(14) . . ?
C221 C22 C222 111.449(3) . . ?
C221 C22 H22 106.7685(10) . . ?
C221 C22 N2 113.7757(18) . . ?
C22 N2 Cr1 114.5981(17) . . ?
C21 N2 Cr1 129.990(2) . . ?
C21 N2 C22 115.400(3) . . ?
C31 N3 Cr1 114.364(2) . . ?
C32 N3 Cr1 130.2375(18) . . ?
C32 N3 C31 115.3633(18) . . ?
H31 C31 N3 106.6410(15) . . ?
C312 C31 N3 110.547(3) . . ?
C312 C31 H31 106.6410(14) . . ?
C311 C31 N3 113.2520(16) . . ?
C311 C31 H31 106.6410(18) . . ?
C311 C31 C312 112.6328(16) . . ?
H31a C312 C31 109.5 . . ?
H31b C312 C31 109.5 . . ?
H31b C312 H31a 109.5 . . ?
H31c C312 C31 109.5 . . ?
H31c C312 H31a 109.5 . . ?
H31c C312 H31b 109.5 . . ?
H31d C311 C31 109.5 . . ?
H31e C311 C31 109.5 . . ?
H31e C311 H31d 109.5 . . ?
H31f C311 C31 109.5 . . ?
H31f C311 H31d 109.5 . . ?
H31f C311 H31e 109.5 . . ?
H22d C221 C22 109.5 . . ?
H22e C221 C22 109.5 . . ?
H22e C221 H22d 109.5 . . ?
H22f C221 C22 109.5 . . ?
H22f C221 H22d 109.5 . . ?
H22f C221 H22e 109.5 . . ?
H21 C21 N2 107.6173(18) . . ?
C212 C21 N2 110.9198(18) . . ?
C212 C21 H21 107.6173(18) . . ?
C211 C21 N2 111.063(2) . . ?
C211 C21 H21 107.6173(17) . . ?
C211 C21 C212 111.7957(19) . . ?
H21a C212 C21 109.5 . . ?
H21b C212 C21 109.5 . . ?
H21b C212 H21a 109.5 . . ?
H21c C212 C21 109.5 . . ?
H21c C212 H21a 109.5 . . ?
H21c C212 H21b 109.5 . . ?
H21d C211 C21 109.5 . . ?
H21e C211 C21 109.5 . . ?
H21e C211 H21d 109.5 . . ?
H21f C211 C21 109.5 . . ?
H21f C211 H21d 109.5 . . ?
H21f C211 H21e 109.5 . . ?
H32 C32 N3 107.7335(10) . . ?
C321 C32 N3 111.275(2) . . ?
C321 C32 H32 107.7335(9) . . ?
C322 C32 N3 111.1847(18) . . ?
C322 C32 H32 107.7335(11) . . ?
C322 C32 C321 110.995(2) . . ?
H32a C321 C32 109.5 . . ?
H32b C321 C32 109.5 . . ?
H32b C321 H32a 109.5 . . ?
H32c C321 C32 109.5 . . ?
H32c C321 H32a 109.5 . . ?
H32c C321 H32b 109.5 . . ?
H32d C322 C32 109.5 . . ?
H32e C322 C32 109.5 . . ?
H32e C322 H32d 109.5 . . ?
H32f C322 C32 109.5 . . ?
H32f C322 H32d 109.5 . . ?
H32f C322 H32e 109.5 . . ?
H3b C3 H3a 109.5 . . ?
H3c C3 H3a 109.5 . . ?
H3c C3 H3b 109.5 . . ?
C1 C3 H3a 109.5 . . ?
C1 C3 H3b 109.5 . . ?
C1 C3 H3c 109.5 . . ?
C4 C1 C3 111.054(2) . . ?
C2 C1 C3 110.177(2) . . ?
C2 C1 C4 110.0872(16) . . ?
S1 C1 C3 111.2038(16) . . ?
S1 C1 C4 104.6479(19) . . ?
S1 C1 C2 109.539(2) . . ?
H4a C4 C1 109.5 . . ?
H4b C4 C1 109.5 . . ?
H4b C4 H4a 109.5 . . ?
H4c C4 C1 109.5 . . ?
H4c C4 H4a 109.5 . . ?
H4c C4 H4b 109.5 . . ?
H2a C2 C1 109.5 . . ?
H2b C2 C1 109.5 . . ?
H2b C2 H2a 109.5 . . ?
H2c C2 C1 109.5 . . ?
H2c C2 H2a 109.5 . . ?
H2c C2 H2b 109.5 . . ?
C1 S1 Cr1 114.1070(15) . . ?

# start Validation Reply Form
_vrf_PLAT230_RDB-1-CrStBu        
;
PROBLEM: Hirshfeld Test Diff for    S1     --  C1      ..       13.5 su    
RESPONSE: Minor disorder that we did not attempt to model.
;
_vrf_PLAT073_RDB-1-CrStBu        
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr       
RESPONSE: Olex2 was used to refine this structure, which provides e.s.d.s
for rider atoms, causing this spurious checkCIF alert.
;
_database_code_depnum_ccdc_archive 'CCDC 1000430'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_RDB-1-131
_audit_creation_date             2014-04-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2900 for OlexSys, GUI svn.r4781)
;
_chemical_formula_moiety         'C16 H37 Cr N3 Se'
_chemical_formula_sum            'C16 H37 Cr N3 Se'
_chemical_formula_weight         402.45
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cr 0.32644 0.61635 10.64060 7.35370 3.32400 1.49220 6.10380 0.39200 20.26260
98.73990 1.18320000172
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Se -0.08110 2.30834 17.00060 5.81960 3.97310 4.35430 2.40980 0.27260 15.23720
43.81630 2.84089994431
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   13.0772(9)
_cell_length_b                   9.4776(7)
_cell_length_c                   17.8289(13)
_cell_angle_alpha                90
_cell_angle_beta                 105.233(1)
_cell_angle_gamma                90
_cell_volume                     2132.1(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8394
_cell_measurement_temperature    173.13
_cell_measurement_theta_max      28.621
_cell_measurement_theta_min      2.239
_exptl_absorpt_coefficient_mu    2.243
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1443 before and 0.0422 after correction.
The Ratio of minimum to maximum transmission is 0.8811.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.2537
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             849.1700
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.365
_exptl_crystal_size_min          0.272
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            20807
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.08
_diffrn_reflns_theta_min         2.24
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9187
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -17
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -11
_reflns_number_gt                3999
_reflns_number_total             5241
_reflns_threshold_expression     I>=2u(I)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_data_collection       cosmo
_computing_structure_solution    shelxT
_refine_diff_density_max         0.9043
_refine_diff_density_min         -0.7422
_refine_diff_density_rms         0.1029
_refine_ls_d_res_high            0.7311
_refine_ls_d_res_low             9.0979
_refine_ls_goodness_of_fit_ref   1.0162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5241
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.0162
_refine_ls_shift/su_max          0.0114
_refine_ls_shift/su_mean         0.0003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0406P)²+0.4707P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0845
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C22(H22), C31(H31), C32(H32)
2.b Idealised Me refined as rotating group:
 C211(H21a,H21b,H21c), C212(H21d,H21e,H21f), C221(H22a,H22b,H22c), C222(H22d,
 H22e,H22f), C312(H31a,H31b,H31c), C311(H31d,H31e,H31f), C321(H32a,H32b,H32c),
 C322(H32d,H32e,H32f), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C2(H2a,H2b,H2c)
;
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_refinement_flags_posn
Se1 Se 0.337501(2) 1.059551(2) -0.068333(2) 0.03898(7) Uani 1.000000 .
Cr1 Cr 0.253222(2) 0.957950(2) 0.022037(2) 0.02184(8) Uani 1.000000 .
N2 N 0.293050(2) 1.050050(2) 0.114360(2) 0.0267(2) Uani 1.000000 .
N3 N 0.266750(2) 0.767250(2) 0.021950(2) 0.0266(2) Uani 1.000000 .
C21 C 0.227880(2) 1.135200(2) 0.153950(2) 0.0384(3) Uani 1.000000 .
H21 H 0.275300(2) 1.169158(2) 0.204245(2) 0.0461(3) Uiso 1.000000 R
C211 C 0.140810(2) 1.047910(2) 0.172610(2) 0.0576(3) Uani 1.000000 .
H21a H 0.092734(2) 1.013624(2) 0.124210(2) 0.0864(4) Uiso 1.000000 GR
H21b H 0.172147(2) 0.967372(2) 0.205042(2) 0.0864(4) Uiso 1.000000 GR
H21c H 0.101170(2) 1.106213(2) 0.200661(2) 0.0864(4) Uiso 1.000000 GR
C212 C 0.183320(2) 1.264870(2) 0.105340(2) 0.0582(3) Uani 1.000000 .
H21d H 0.241063(2) 1.315641(2) 0.091510(2) 0.0873(4) Uiso 1.000000 GR
H21e H 0.131022(2) 1.235016(2) 0.057850(2) 0.0873(4) Uiso 1.000000 GR
H21f H 0.149301(2) 1.327103(2) 0.135489(2) 0.0873(4) Uiso 1.000000 GR
C22 C 0.405590(2) 1.038880(2) 0.155880(2) 0.0348(3) Uani 1.000000 .
H22 H 0.439411(2) 0.977839(2) 0.123409(2) 0.0418(3) Uiso 1.000000 R
C221 C 0.423780(2) 0.966990(2) 0.234220(2) 0.0573(3) Uani 1.000000 .
H22a H 0.398580(2) 1.028280(2) 0.269883(2) 0.0859(4) Uiso 1.000000 GR
H22b H 0.384873(2) 0.877529(2) 0.227986(2) 0.0859(4) Uiso 1.000000 GR
H22c H 0.499649(2) 0.948677(2) 0.255447(2) 0.0859(4) Uiso 1.000000 GR
C222 C 0.459630(2) 1.182760(2) 0.161510(2) 0.0568(3) Uani 1.000000 .
H22d H 0.445809(2) 1.224759(2) 0.109580(2) 0.0852(4) Uiso 1.000000 GR
H22e H 0.431569(2) 1.244661(2) 0.195399(2) 0.0852(4) Uiso 1.000000 GR
H22f H 0.536193(2) 1.171200(2) 0.183165(2) 0.0852(4) Uiso 1.000000 GR
N1 N 0.133970(2) 0.987850(2) -0.008880(2) 0.0312(2) Uani 1.000000 .
C31 C 0.184160(2) 0.657080(2) 0.006000(2) 0.0352(3) Uani 1.000000 .
H31 H 0.220336(2) 0.563233(2) 0.014259(2) 0.0423(3) Uiso 1.000000 R
C312 C 0.117920(2) 0.663500(2) -0.077400(2) 0.0469(3) Uani 1.000000 .
H31a H 0.079340(2) 0.753193(2) -0.086419(2) 0.0704(4) Uiso 1.000000 GR
H31b H 0.164249(2) 0.656339(2) -0.112424(2) 0.0704(4) Uiso 1.000000 GR
H31c H 0.067257(2) 0.585127(2) -0.087389(2) 0.0704(4) Uiso 1.000000 GR
C311 C 0.115820(2) 0.669290(2) 0.062970(2) 0.0566(3) Uani 1.000000 .
H31d H 0.161048(2) 0.664680(2) 0.116305(2) 0.0849(4) Uiso 1.000000 GR
H31e H 0.077834(2) 0.759472(2) 0.054996(2) 0.0849(4) Uiso 1.000000 GR
H31f H 0.064616(2) 0.591572(2) 0.054258(2) 0.0849(4) Uiso 1.000000 GR
C32 C 0.377040(2) 0.715560(2) 0.037980(2) 0.0352(3) Uani 1.000000 .
H32 H 0.423814(2) 0.800729(2) 0.047603(2) 0.0422(3) Uiso 1.000000 R
C321 C 0.410170(2) 0.624500(2) 0.110580(2) 0.0539(3) Uani 1.000000 .
H32a H 0.396031(2) 0.675197(2) 0.154705(2) 0.0809(4) Uiso 1.000000 GR
H32b H 0.369784(2) 0.536183(2) 0.102202(2) 0.0809(4) Uiso 1.000000 GR
H32c H 0.486042(2) 0.603446(2) 0.121612(2) 0.0809(4) Uiso 1.000000 GR
C322 C 0.395740(2) 0.641960(2) -0.033330(2) 0.0508(3) Uani 1.000000 .
H32d H 0.357238(2) 0.552170(2) -0.041558(2) 0.0762(4) Uiso 1.000000 GR
H32e H 0.370301(2) 0.702287(2) -0.079084(2) 0.0762(4) Uiso 1.000000 GR
H32f H 0.471696(2) 0.624131(2) -0.025168(2) 0.0762(4) Uiso 1.000000 GR
C1 C 0.227210(2) 1.146140(2) -0.155480(2) 0.0340(3) Uani 1.000000 .
C3 C 0.286310(2) 1.189660(2) -0.214470(2) 0.0856(3) Uani 1.000000 .
H3a H 0.343114(2) 1.255615(2) -0.190256(2) 0.1284(4) Uiso 1.000000 GR
H3b H 0.316908(2) 1.105936(2) -0.232483(2) 0.1284(4) Uiso 1.000000 GR
H3c H 0.237093(2) 1.235547(2) -0.258785(2) 0.1284(4) Uiso 1.000000 GR
C4 C 0.142860(2) 1.040460(2) -0.191480(2) 0.0530(3) Uani 1.000000 .
H4a H 0.175832(2) 0.956974(2) -0.207649(2) 0.0795(4) Uiso 1.000000 GR
H4b H 0.104526(2) 1.012876(2) -0.153366(2) 0.0795(4) Uiso 1.000000 GR
H4c H 0.093233(2) 1.082636(2) -0.236893(2) 0.0795(4) Uiso 1.000000 GR
C2 C 0.178820(2) 1.270890(2) -0.125670(2) 0.0813(3) Uani 1.000000 .
H2a H 0.143065(2) 1.239256(2) -0.086754(2) 0.1220(5) Uiso 1.000000 GR
H2b H 0.234581(2) 1.338572(2) -0.101902(2) 0.1220(5) Uiso 1.000000 GR
H2c H 0.127252(2) 1.316209(2) -0.168911(2) 0.1220(5) Uiso 1.000000 GR


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
Se1 Cr1 2.38139(12) . ?
Se1 C1 1.99755(10) . ?
Cr1 N2 1.81441(12) . ?
Cr1 N3 1.81606(14) . ?
Cr1 N1 1.53767(11) . ?
N2 C21 1.48051(8) . ?
N2 C22 1.46718(10) . ?
N3 C31 1.47520(8) . ?
N3 C32 1.47826(10) . ?
C21 H21 1.0000 . ?
C21 C211 1.51349(9) . ?
C21 C212 1.52828(9) . ?
C211 H21a 0.9800 . ?
C211 H21b 0.9800 . ?
C211 H21c 0.9800 . ?
C212 H21d 0.9800 . ?
C212 H21e 0.9800 . ?
C212 H21f 0.9800 . ?
C22 H22 1.0000 . ?
C22 C221 1.51560(11) . ?
C22 C222 1.52700(10) . ?
C221 H22a 0.9800 . ?
C221 H22b 0.9800 . ?
C221 H22c 0.9800 . ?
C222 H22d 0.9800 . ?
C222 H22e 0.9800 . ?
C222 H22f 0.9800 . ?
C31 H31 1.0000 . ?
C31 C312 1.51268(11) . ?
C31 C311 1.52340(10) . ?
C312 H31a 0.9800 . ?
C312 H31b 0.9800 . ?
C312 H31c 0.9800 . ?
C311 H31d 0.9800 . ?
C311 H31e 0.9800 . ?
C311 H31f 0.9800 . ?
C32 H32 1.0000 . ?
C32 C321 1.52094(10) . ?
C32 C322 1.52517(10) . ?
C321 H32a 0.9800 . ?
C321 H32b 0.9800 . ?
C321 H32c 0.9800 . ?
C322 H32d 0.9800 . ?
C322 H32e 0.9800 . ?
C322 H32f 0.9800 . ?
C1 C3 1.51681(10) . ?
C1 C4 1.50328(8) . ?
C1 C2 1.50252(9) . ?
C3 H3a 0.9800 . ?
C3 H3b 0.9800 . ?
C3 H3c 0.9800 . ?
C4 H4a 0.9800 . ?
C4 H4b 0.9800 . ?
C4 H4c 0.9800 . ?
C2 H2a 0.9800 . ?
C2 H2b 0.9800 . ?
C2 H2c 0.9800 . ?

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
C1 Se1 Cr1 108.932(2) . . ?
N2 Cr1 Se1 110.2242(19) . . ?
N3 Cr1 Se1 109.837(2) . . ?
N3 Cr1 N2 118.343(3) . . ?
N1 Cr1 Se1 106.800(3) . . ?
N1 Cr1 N2 105.004(3) . . ?
N1 Cr1 N3 105.840(2) . . ?
C21 N2 Cr1 129.106(3) . . ?
C22 N2 Cr1 115.709(3) . . ?
C22 N2 C21 115.185(3) . . ?
C31 N3 Cr1 129.645(2) . . ?
C32 N3 Cr1 114.832(2) . . ?
C32 N3 C31 115.494(2) . . ?
H21 C21 N2 107.6929(18) . . ?
C211 C21 N2 111.555(2) . . ?
C211 C21 H21 107.693(2) . . ?
C212 C21 N2 110.454(4) . . ?
C212 C21 H21 107.6929(17) . . ?
C212 C21 C211 111.557(3) . . ?
H21a C211 C21 109.5 . . ?
H21b C211 C21 109.5 . . ?
H21b C211 H21a 109.5 . . ?
H21c C211 C21 109.5 . . ?
H21c C211 H21a 109.5 . . ?
H21c C211 H21b 109.5 . . ?
H21d C212 C21 109.5 . . ?
H21e C212 C21 109.5 . . ?
H21e C212 H21d 109.5 . . ?
H21f C212 C21 109.5 . . ?
H21f C212 H21d 109.5 . . ?
H21f C212 H21e 109.5 . . ?
H22 C22 N2 106.693(2) . . ?
C221 C22 N2 113.026(3) . . ?
C221 C22 H22 106.6928(18) . . ?
C222 C22 N2 110.749(2) . . ?
C222 C22 H22 106.693(2) . . ?
C222 C22 C221 112.521(3) . . ?
H22a C221 C22 109.5 . . ?
H22b C221 C22 109.5 . . ?
H22b C221 H22a 109.5 . . ?
H22c C221 C22 109.5 . . ?
H22c C221 H22a 109.5 . . ?
H22c C221 H22b 109.5 . . ?
H22d C222 C22 109.5 . . ?
H22e C222 C22 109.5 . . ?
H22e C222 H22d 109.5 . . ?
H22f C222 C22 109.5 . . ?
H22f C222 H22d 109.5 . . ?
H22f C222 H22e 109.5 . . ?
H31 C31 N3 107.8842(15) . . ?
C312 C31 N3 111.234(3) . . ?
C312 C31 H31 107.8842(14) . . ?
C311 C31 N3 110.228(3) . . ?
C311 C31 H31 107.8842(14) . . ?
C311 C31 C312 111.567(3) . . ?
H31a C312 C31 109.5 . . ?
H31b C312 C31 109.5 . . ?
H31b C312 H31a 109.5 . . ?
H31c C312 C31 109.5 . . ?
H31c C312 H31a 109.5 . . ?
H31c C312 H31b 109.5 . . ?
H31d C311 C31 109.5 . . ?
H31e C311 C31 109.5 . . ?
H31e C311 H31d 109.5 . . ?
H31f C311 C31 109.5 . . ?
H31f C311 H31d 109.5 . . ?
H31f C311 H31e 109.5 . . ?
H32 C32 N3 106.7019(13) . . ?
C321 C32 N3 113.445(3) . . ?
C321 C32 H32 106.7019(15) . . ?
C322 C32 N3 110.634(3) . . ?
C322 C32 H32 106.7019(16) . . ?
C322 C32 C321 112.191(2) . . ?
H32a C321 C32 109.5 . . ?
H32b C321 C32 109.5 . . ?
H32b C321 H32a 109.5 . . ?
H32c C321 C32 109.5 . . ?
H32c C321 H32a 109.5 . . ?
H32c C321 H32b 109.5 . . ?
H32d C322 C32 109.5 . . ?
H32e C322 C32 109.5 . . ?
H32e C322 H32d 109.5 . . ?
H32f C322 C32 109.5 . . ?
H32f C322 H32d 109.5 . . ?
H32f C322 H32e 109.5 . . ?
C3 C1 Se1 104.817(2) . . ?
C4 C1 Se1 110.930(2) . . ?
C4 C1 C3 109.605(3) . . ?
C2 C1 Se1 109.468(3) . . ?
C2 C1 C3 111.714(2) . . ?
C2 C1 C4 110.202(3) . . ?
H3a C3 C1 109.5 . . ?
H3b C3 C1 109.5 . . ?
H3b C3 H3a 109.5 . . ?
H3c C3 C1 109.5 . . ?
H3c C3 H3a 109.5 . . ?
H3c C3 H3b 109.5 . . ?
H4a C4 C1 109.5 . . ?
H4b C4 C1 109.5 . . ?
H4b C4 H4a 109.5 . . ?
H4c C4 C1 109.5 . . ?
H4c C4 H4a 109.5 . . ?
H4c C4 H4b 109.5 . . ?
H2a C2 C1 109.5 . . ?
H2b C2 C1 109.5 . . ?
H2b C2 H2a 109.5 . . ?
H2c C2 C1 109.5 . . ?
H2c C2 H2a 109.5 . . ?
H2c C2 H2b 109.5 . . ?

# start Validation Reply Form
_vrf_PLAT230_RDB-1-131           
;
PROBLEM: Hirshfeld Test Diff for    Se1    --  C1      ..        7.5 su    
RESPONSE: Minor disorder that we did not attempt to model.
;
_vrf_PLAT073_RDB-1-131           
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr       
RESPONSE: Olex2 was used to refine this structure, which provides e.s.d.s
for rider atoms, causing this spurious checkCIF alert.
;
_database_code_depnum_ccdc_archive 'CCDC 1000431'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_rbd-1-127c
_audit_creation_date             2014-04-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.02.28 svn.r2900 for OlexSys, GUI svn.r4781)
;
_chemical_formula_moiety         'C16 H37 Cr N3 Te'
_chemical_formula_sum            'C16 H37 Cr N3 Te'
_chemical_formula_weight         451.09
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Cr 0.32644 0.61635 10.64060 7.35370 3.32400 1.49220 6.10380 0.39200 20.26260
98.73990 1.18320000172
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Te -0.41596 1.76393 19.96440 19.01380 6.14487 2.52390 4.81742 0.42088 28.52840
70.84030 4.35200023651
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x+1/2,y+1/2,-z+1/2
3 -x,-y,-z
4 x-1/2,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   13.1606(12)
_cell_length_b                   9.5014(8)
_cell_length_c                   18.0100(16)
_cell_angle_alpha                90
_cell_angle_beta                 103.494(1)
_cell_angle_gamma                90
_cell_volume                     2189.9(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8975
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.18
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1132 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.8425.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.3681
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             919.8407
_exptl_crystal_preparation       ?
_exptl_crystal_recrystallization_method 'cold pentane'
_exptl_crystal_size_max          0.503
_exptl_crystal_size_mid          0.211
_exptl_crystal_size_min          0.193
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21407
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         29.14
_diffrn_reflns_theta_min         2.18
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.9992
_diffrn_measured_fraction_theta_max 0.9305
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_special_details          ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -17
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -12
_reflns_number_gt                4204
_reflns_number_total             5472
_reflns_threshold_expression     I>=2u(I)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_data_collection       cosmo
_computing_structure_solution    shelxT
_refine_diff_density_max         1.0494
_refine_diff_density_min         -0.7149
_refine_diff_density_rms         0.1237
_refine_ls_d_res_high            0.7297
_refine_ls_d_res_low             9.3458
_refine_ls_goodness_of_fit_ref   1.0053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     200
_refine_ls_number_reflns         5472
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0342
_refine_ls_restrained_S_all      1.0053
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0314P)²+1.7555P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0803
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C21(H21), C22(H22), C32(H32), C31(H31)
2.b Idealised Me refined as rotating group:
 C212(H21a,H21b,H21c), C211(H21d,H21e,H21f), C222(H22a,H22b,H22c), C221(H22d,
 H22e,H22f), C321(H32a,H32b,H32c), C322(H32d,H32e,H32f), C311(H31a,H31b,H31c),
 C312(H31d,H31e,H31f), C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c)
;
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_refinement_flags_posn
Te1 Te 0.654551(14) 0.43101(2) 1.071789(11) 0.04340(8) Uani 1.000000 .
Cr1 Cr 0.75005(2) 0.54151(3) 0.975876(19) 0.02435(10) Uani 1.000000 .
N1 N 0.86637(3) 0.50844(3) 1.00905(3) 0.0323(5) Uani 1.000000 .
N2 N 0.71530(3) 0.44673(3) 0.88577(3) 0.0300(5) Uani 1.000000 .
N3 N 0.73804(3) 0.73169(3) 0.97734(3) 0.0296(5) Uani 1.000000 .
C21 C 0.78261(3) 0.36025(3) 0.84853(3) 0.0414(7) Uani 1.000000 .
H21 H 0.73858(3) 0.32569(3) 0.79893(3) 0.0497(8) Uiso 1.000000 R
C212 C 0.82260(3) 0.23254(3) 0.89721(3) 0.0591(9) Uani 1.000000 .
H21a H 0.87088(3) 0.26298(3) 0.94450(3) 0.0886(14) Uiso 1.000000 GR
H21b H 0.76357(3) 0.18244(3) 0.90958(3) 0.0886(14) Uiso 1.000000 GR
H21c H 0.85916(3) 0.16973(3) 0.86898(3) 0.0886(14) Uiso 1.000000 GR
C211 C 0.87052(3) 0.44679(3) 0.83098(3) 0.0595(9) Uani 1.000000 .
H21d H 0.84131(3) 0.52575(3) 0.79781(3) 0.0892(14) Uiso 1.000000 GR
H21e H 0.91462(3) 0.48301(3) 0.87867(3) 0.0892(14) Uiso 1.000000 GR
H21f H 0.91263(3) 0.38771(3) 0.80508(3) 0.0892(14) Uiso 1.000000 GR
C22 C 0.60483(3) 0.45746(3) 0.84425(3) 0.0400(7) Uani 1.000000 .
H22 H 0.56939(3) 0.51844(3) 0.87581(3) 0.0480(8) Uiso 1.000000 R
C222 C 0.55186(3) 0.31431(3) 0.83881(3) 0.0599(9) Uani 1.000000 .
H22a H 0.57827(3) 0.25451(3) 0.80314(3) 0.0899(14) Uiso 1.000000 GR
H22b H 0.56700(3) 0.27002(3) 0.88934(3) 0.0899(14) Uiso 1.000000 GR
H22c H 0.47618(3) 0.32617(3) 0.82044(3) 0.0899(14) Uiso 1.000000 GR
C221 C 0.59056(3) 0.52876(3) 0.76713(3) 0.0683(10) Uani 1.000000 .
H22d H 0.63076(3) 0.61652(3) 0.77296(3) 0.1025(15) Uiso 1.000000 GR
H22e H 0.61532(3) 0.46612(3) 0.73186(3) 0.1025(15) Uiso 1.000000 GR
H22f H 0.51637(3) 0.54968(3) 0.74674(3) 0.1025(15) Uiso 1.000000 GR
C32 C 0.62965(3) 0.78520(3) 0.95828(3) 0.0444(8) Uani 1.000000 .
H32 H 0.58318(3) 0.70082(3) 0.94710(3) 0.0533(9) Uiso 1.000000 R
C321 C 0.60409(3) 0.87615(3) 0.88737(3) 0.0708(12) Uani 1.000000 .
H32a H 0.63829(3) 0.96788(3) 0.89856(3) 0.1062(18) Uiso 1.000000 GR
H32b H 0.62915(3) 0.83005(3) 0.84634(3) 0.1062(18) Uiso 1.000000 GR
H32c H 0.52828(3) 0.88943(3) 0.87129(3) 0.1062(18) Uiso 1.000000 GR
C322 C 0.60345(3) 0.85810(3) 1.02737(3) 0.0603(10) Uani 1.000000 .
H32d H 0.62412(3) 0.79735(3) 1.07234(3) 0.0904(15) Uiso 1.000000 GR
H32e H 0.64136(3) 0.94753(3) 1.03696(3) 0.0904(15) Uiso 1.000000 GR
H32f H 0.52812(3) 0.87605(3) 1.01700(3) 0.0904(15) Uiso 1.000000 GR
C31 C 0.82056(3) 0.83982(3) 0.99608(3) 0.0368(6) Uani 1.000000 .
H31 H 0.78605(3) 0.93415(3) 0.98788(3) 0.0442(8) Uiso 1.000000 R
C311 C 0.89425(3) 0.82829(3) 0.94256(3) 0.0587(9) Uani 1.000000 .
H31a H 0.93099(3) 0.73786(3) 0.95070(3) 0.0880(14) Uiso 1.000000 GR
H31b H 0.85398(3) 0.83438(3) 0.88953(3) 0.0880(14) Uiso 1.000000 GR
H31c H 0.94522(3) 0.90520(3) 0.95301(3) 0.0880(14) Uiso 1.000000 GR
C312 C 0.87896(3) 0.83075(3) 1.07885(3) 0.0467(8) Uani 1.000000 .
H31d H 0.82934(3) 0.83812(3) 1.11165(3) 0.0700(11) Uiso 1.000000 GR
H31e H 0.91572(3) 0.74043(3) 1.08801(3) 0.0700(11) Uiso 1.000000 GR
H31f H 0.92968(3) 0.90781(3) 1.09054(3) 0.0700(11) Uiso 1.000000 GR
C1 C 0.77700(3) 0.33630(3) 1.16214(3) 0.0360(6) Uani 1.000000 .
C2 C 0.86065(3) 0.44180(3) 1.19293(3) 0.0637(11) Uani 1.000000 .
H2a H 0.89262(3) 0.47334(3) 1.15182(3) 0.0956(16) Uiso 1.000000 GR
H2b H 0.83000(3) 0.52267(3) 1.21352(3) 0.0956(16) Uiso 1.000000 GR
H2c H 0.91410(3) 0.39849(3) 1.23360(3) 0.0956(16) Uiso 1.000000 GR
C3 C 0.82338(3) 0.21297(3) 1.13033(3) 0.0979(15) Uani 1.000000 .
H3a H 0.76792(3) 0.14619(3) 1.10797(3) 0.147(2) Uiso 1.000000 GR
H3b H 0.85810(3) 0.24530(3) 1.09085(3) 0.147(2) Uiso 1.000000 GR
H3c H 0.87451(3) 0.16660(3) 1.17134(3) 0.147(2) Uiso 1.000000 GR
C4 C 0.72256(3) 0.29389(3) 1.22371(3) 0.1000(13) Uani 1.000000 .
H4a H 0.69271(3) 0.37749(3) 1.24241(3) 0.1501(19) Uiso 1.000000 GR
H4b H 0.66659(3) 0.22691(3) 1.20274(3) 0.1501(19) Uiso 1.000000 GR
H4c H 0.77301(3) 0.24973(3) 1.26597(3) 0.1501(19) Uiso 1.000000 GR


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
Te1 Cr1 2.5843(4) . ?
Te1 C1 2.1980(5) . ?
Cr1 N1 1.5403(5) . ?
Cr1 N2 1.8186(6) . ?
Cr1 N3 1.8146(4) . ?
N2 C21 1.4788(7) . ?
N2 C22 1.4751(6) . ?
N3 C32 1.4773(6) . ?
N3 C31 1.4757(5) . ?
C21 H21 1.0000 . ?
C21 C212 1.5174(6) . ?
C21 C211 1.5118(6) . ?
C212 H21a 0.9800 . ?
C212 H21b 0.9800 . ?
C212 H21c 0.9800 . ?
C211 H21d 0.9800 . ?
C211 H21e 0.9800 . ?
C211 H21f 0.9800 . ?
C22 H22 1.0000 . ?
C22 C222 1.5211(5) . ?
C22 C221 1.5172(8) . ?
C222 H22a 0.9800 . ?
C222 H22b 0.9800 . ?
C222 H22c 0.9800 . ?
C221 H22d 0.9800 . ?
C221 H22e 0.9800 . ?
C221 H22f 0.9800 . ?
C32 H32 1.0000 . ?
C32 C321 1.5133(7) . ?
C32 C322 1.5321(8) . ?
C321 H32a 0.9800 . ?
C321 H32b 0.9800 . ?
C321 H32c 0.9800 . ?
C322 H32d 0.9800 . ?
C322 H32e 0.9800 . ?
C322 H32f 0.9800 . ?
C31 H31 1.0000 . ?
C31 C311 1.5224(8) . ?
C31 C312 1.5118(7) . ?
C311 H31a 0.9800 . ?
C311 H31b 0.9800 . ?
C311 H31c 0.9800 . ?
C312 H31d 0.9800 . ?
C312 H31e 0.9800 . ?
C312 H31f 0.9800 . ?
C1 C2 1.4964(5) . ?
C1 C3 1.4957(6) . ?
C1 C4 1.5086(8) . ?
C2 H2a 0.9800 . ?
C2 H2b 0.9800 . ?
C2 H2c 0.9800 . ?
C3 H3a 0.9800 . ?
C3 H3b 0.9800 . ?
C3 H3c 0.9800 . ?
C4 H4a 0.9800 . ?
C4 H4b 0.9800 . ?
C4 H4c 0.9800 . ?

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
C1 Te1 Cr1 105.918(16) . . ?
N1 Cr1 Te1 104.61(2) . . ?
N2 Cr1 Te1 109.575(19) . . ?
N2 Cr1 N1 105.38(3) . . ?
N3 Cr1 Te1 109.71(2) . . ?
N3 Cr1 N1 106.24(2) . . ?
N3 Cr1 N2 120.10(3) . . ?
C21 N2 Cr1 128.85(3) . . ?
C22 N2 Cr1 115.53(4) . . ?
C22 N2 C21 115.61(4) . . ?
C32 N3 Cr1 114.96(3) . . ?
C31 N3 Cr1 129.39(3) . . ?
C31 N3 C32 115.64(3) . . ?
H21 C21 N2 107.70(2) . . ?
C212 C21 N2 110.24(5) . . ?
C212 C21 H21 107.70(2) . . ?
C211 C21 N2 111.18(3) . . ?
C211 C21 H21 107.70(3) . . ?
C211 C21 C212 112.12(3) . . ?
H21a C212 C21 109.5 . . ?
H21b C212 C21 109.5 . . ?
H21b C212 H21a 109.5 . . ?
H21c C212 C21 109.5 . . ?
H21c C212 H21a 109.5 . . ?
H21c C212 H21b 109.5 . . ?
H21d C211 C21 109.5 . . ?
H21e C211 C21 109.5 . . ?
H21e C211 H21d 109.5 . . ?
H21f C211 C21 109.5 . . ?
H21f C211 H21d 109.5 . . ?
H21f C211 H21e 109.5 . . ?
H22 C22 N2 106.69(3) . . ?
C222 C22 N2 110.71(3) . . ?
C222 C22 H22 106.69(3) . . ?
C221 C22 N2 113.07(4) . . ?
C221 C22 H22 106.69(2) . . ?
C221 C22 C222 112.54(4) . . ?
H22a C222 C22 109.5 . . ?
H22b C222 C22 109.5 . . ?
H22b C222 H22a 109.5 . . ?
H22c C222 C22 109.5 . . ?
H22c C222 H22a 109.5 . . ?
H22c C222 H22b 109.5 . . ?
H22d C221 C22 109.5 . . ?
H22e C221 C22 109.5 . . ?
H22e C221 H22d 109.5 . . ?
H22f C221 C22 109.5 . . ?
H22f C221 H22d 109.5 . . ?
H22f C221 H22e 109.5 . . ?
H32 C32 N3 106.434(17) . . ?
C321 C32 N3 113.90(4) . . ?
C321 C32 H32 106.43(2) . . ?
C322 C32 N3 110.79(4) . . ?
C322 C32 H32 106.43(2) . . ?
C322 C32 C321 112.29(3) . . ?
H32a C321 C32 109.5 . . ?
H32b C321 C32 109.5 . . ?
H32b C321 H32a 109.5 . . ?
H32c C321 C32 109.5 . . ?
H32c C321 H32a 109.5 . . ?
H32c C321 H32b 109.5 . . ?
H32d C322 C32 109.5 . . ?
H32e C322 C32 109.5 . . ?
H32e C322 H32d 109.5 . . ?
H32f C322 C32 109.5 . . ?
H32f C322 H32d 109.5 . . ?
H32f C322 H32e 109.5 . . ?
H31 C31 N3 107.79(2) . . ?
C311 C31 N3 110.41(4) . . ?
C311 C31 H31 107.790(18) . . ?
C312 C31 N3 111.31(4) . . ?
C312 C31 H31 107.790(19) . . ?
C312 C31 C311 111.57(4) . . ?
H31a C311 C31 109.5 . . ?
H31b C311 C31 109.5 . . ?
H31b C311 H31a 109.5 . . ?
H31c C311 C31 109.5 . . ?
H31c C311 H31a 109.5 . . ?
H31c C311 H31b 109.5 . . ?
H31d C312 C31 109.5 . . ?
H31e C312 C31 109.5 . . ?
H31e C312 H31d 109.5 . . ?
H31f C312 C31 109.5 . . ?
H31f C312 H31d 109.5 . . ?
H31f C312 H31e 109.5 . . ?
C2 C1 Te1 110.42(2) . . ?
C3 C1 Te1 109.36(3) . . ?
C3 C1 C2 109.64(4) . . ?
C4 C1 Te1 105.16(3) . . ?
C4 C1 C2 109.94(4) . . ?
C4 C1 C3 112.24(3) . . ?
H2a C2 C1 109.5 . . ?
H2b C2 C1 109.5 . . ?
H2b C2 H2a 109.5 . . ?
H2c C2 C1 109.5 . . ?
H2c C2 H2a 109.5 . . ?
H2c C2 H2b 109.5 . . ?
H3a C3 C1 109.5 . . ?
H3b C3 C1 109.5 . . ?
H3b C3 H3a 109.5 . . ?
H3c C3 C1 109.5 . . ?
H3c C3 H3a 109.5 . . ?
H3c C3 H3b 109.5 . . ?
H4a C4 C1 109.5 . . ?
H4b C4 C1 109.5 . . ?
H4b C4 H4a 109.5 . . ?
H4c C4 C1 109.5 . . ?
H4c C4 H4a 109.5 . . ?
H4c C4 H4b 109.5 . . ?
_database_code_depnum_ccdc_archive 'CCDC 1000432'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_aks02212013_0m
_audit_creation_date             2014-02-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H33 Cr N3 Te'
_chemical_formula_sum            'C18 H33 Cr N3 Te'
_chemical_formula_weight         471.07
_chemical_melting_point          ?
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'
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'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.3363(10)
_cell_length_b                   12.2722(15)
_cell_length_c                   21.057(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.7990(10)
_cell_angle_gamma                90
_cell_volume                     2139.1(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.424
_cell_measurement_theta_min      2.559
_shelx_estimated_absorpt_T_max   0.789
_shelx_estimated_absorpt_T_min   0.734
_exptl_absorpt_coefficient_mu    1.875
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0771 before and 0.0673 after correction.
The Ratio of minimum to maximum transmission is 0.7629.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       chunk
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.133
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34480
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.426
_diffrn_reflns_theta_min         1.924
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3518
_reflns_number_total             3930
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_data_collection       cosmo
_computing_structure_solution    shelxT
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.076
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0242
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0320P)²+1.3273P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0639
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1), C4(H4), C7(H7), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Te1 Te 0.20050(2) 0.46357(2) 0.08832(2) 0.02649(7) Uani 1 1 d . . . . .
Cr1 Cr 0.31377(4) 0.26514(3) 0.08593(2) 0.01727(10) Uani 1 1 d . . . . .
N1 N 0.3051(2) 0.23994(15) 0.00053(9) 0.0192(4) Uani 1 1 d . . . . .
N2 N 0.1894(2) 0.18899(17) 0.11176(10) 0.0241(4) Uani 1 1 d . . . . .
N3 N 0.4996(2) 0.24666(15) 0.13925(9) 0.0193(4) Uani 1 1 d . . . . .
C1 C 0.1958(3) 0.1646(2) -0.03910(11) 0.0239(5) Uani 1 1 d . . . . .
H1 H 0.2232 0.1689 -0.0840 0.029 Uiso 1 1 calc R . . . .
C2 C 0.0204(3) 0.2000(2) -0.03962(14) 0.0342(6) Uani 1 1 d . . . . .
H2A H -0.0121 0.1916 0.0033 0.051 Uiso 1 1 calc GR . . . .
H2B H -0.0488 0.1547 -0.0698 0.051 Uiso 1 1 calc GR . . . .
H2C H 0.0094 0.2765 -0.0527 0.051 Uiso 1 1 calc GR . . . .
C3 C 0.2214(4) 0.0475(2) -0.01664(14) 0.0341(6) Uani 1 1 d . . . . .
H3A H 0.3355 0.0280 -0.0164 0.051 Uiso 1 1 calc GR . . . .
H3B H 0.1547 -0.0012 -0.0457 0.051 Uiso 1 1 calc GR . . . .
H3C H 0.1906 0.0401 0.0266 0.051 Uiso 1 1 calc GR . . . .
C4 C 0.4222(3) 0.2983(2) -0.03515(11) 0.0229(5) Uani 1 1 d . . . . .
H4 H 0.4922 0.3431 -0.0032 0.027 Uiso 1 1 calc R . . . .
C5 C 0.5336(3) 0.2220(2) -0.06636(13) 0.0320(6) Uani 1 1 d . . . . .
H5A H 0.5820 0.1695 -0.0346 0.048 Uiso 1 1 calc GR . . . .
H5B H 0.6191 0.2645 -0.0829 0.048 Uiso 1 1 calc GR . . . .
H5C H 0.4713 0.1829 -0.1016 0.048 Uiso 1 1 calc GR . . . .
C6 C 0.3355(3) 0.3775(2) -0.08347(12) 0.0318(6) Uani 1 1 d . . . . .
H6A H 0.2688 0.3365 -0.1167 0.048 Uiso 1 1 calc GR . . . .
H6B H 0.4155 0.4207 -0.1031 0.048 Uiso 1 1 calc GR . . . .
H6C H 0.2666 0.4262 -0.0617 0.048 Uiso 1 1 calc GR . . . .
C7 C 0.6308(3) 0.3239(2) 0.12820(11) 0.0235(5) Uani 1 1 d . . . . .
H7 H 0.5837 0.3770 0.0951 0.028 Uiso 1 1 calc R . . . .
C8 C 0.7724(3) 0.2683(2) 0.10128(14) 0.0342(6) Uani 1 1 d . . . . .
H8A H 0.8250 0.2175 0.1331 0.051 Uiso 1 1 calc GR . . . .
H8B H 0.8505 0.3235 0.0912 0.051 Uiso 1 1 calc GR . . . .
H8C H 0.7325 0.2284 0.0623 0.051 Uiso 1 1 calc GR . . . .
C9 C 0.6826(3) 0.3894(2) 0.18860(13) 0.0332(6) Uani 1 1 d . . . . .
H9A H 0.5887 0.4272 0.2020 0.050 Uiso 1 1 calc GR . . . .
H9B H 0.7645 0.4429 0.1799 0.050 Uiso 1 1 calc GR . . . .
H9C H 0.7281 0.3401 0.2227 0.050 Uiso 1 1 calc GR . . . .
C10 C 0.5469(3) 0.1623(2) 0.18797(11) 0.0247(5) Uani 1 1 d . . . . .
H10 H 0.6651 0.1708 0.2018 0.030 Uiso 1 1 calc R . . . .
C11 C 0.5203(4) 0.0486(2) 0.16014(15) 0.0373(7) Uani 1 1 d . . . . .
H11A H 0.4043 0.0358 0.1492 0.056 Uiso 1 1 calc GR . . . .
H11B H 0.5647 -0.0054 0.1917 0.056 Uiso 1 1 calc GR . . . .
H11C H 0.5748 0.0422 0.1215 0.056 Uiso 1 1 calc GR . . . .
C12 C 0.4591(3) 0.1767(2) 0.24689(13) 0.0351(6) Uani 1 1 d . . . . .
H12A H 0.4708 0.2522 0.2619 0.053 Uiso 1 1 calc GR . . . .
H12B H 0.5057 0.1274 0.2807 0.053 Uiso 1 1 calc GR . . . .
H12C H 0.3442 0.1598 0.2359 0.053 Uiso 1 1 calc GR . . . .
C13 C 0.1310(3) 0.4785(2) 0.18161(12) 0.0232(5) Uani 1 1 d . . . . .
C14 C 0.0732(3) 0.5790(2) 0.20021(13) 0.0291(6) Uani 1 1 d . . . . .
H14 H 0.0728 0.6399 0.1723 0.035 Uiso 1 1 calc R . . . .
C15 C 0.0167(3) 0.5903(2) 0.25882(14) 0.0342(6) Uani 1 1 d . . . . .
H15 H -0.0229 0.6590 0.2708 0.041 Uiso 1 1 calc R . . . .
C16 C 0.0169(3) 0.5036(3) 0.30025(13) 0.0356(6) Uani 1 1 d . . . . .
H16 H -0.0226 0.5119 0.3405 0.043 Uiso 1 1 calc R . . . .
C17 C 0.0755(3) 0.4040(2) 0.28250(13) 0.0328(6) Uani 1 1 d . . . . .
H17 H 0.0767 0.3436 0.3108 0.039 Uiso 1 1 calc R . . . .
C18 C 0.1326(3) 0.3918(2) 0.22338(12) 0.0257(5) Uani 1 1 d . . . . .
H18 H 0.1730 0.3231 0.2117 0.031 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 Cr1 2.6144(5) . ?
Te1 C13 2.121(3) . ?
Cr1 N1 1.8176(19) . ?
Cr1 N2 1.542(2) . ?
Cr1 N3 1.8165(19) . ?
N1 C1 1.484(3) . ?
N1 C4 1.485(3) . ?
N3 C7 1.487(3) . ?
N3 C10 1.477(3) . ?
C1 H1 1.0000 . ?
C1 C2 1.524(3) . ?
C1 C3 1.520(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4 1.0000 . ?
C4 C5 1.521(3) . ?
C4 C6 1.526(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C8 1.529(3) . ?
C7 C9 1.523(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10 1.0000 . ?
C10 C11 1.520(4) . ?
C10 C12 1.523(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 C14 1.398(4) . ?
C13 C18 1.380(4) . ?
C14 H14 0.9500 . ?
C14 C15 1.379(4) . ?
C15 H15 0.9500 . ?
C15 C16 1.376(4) . ?
C16 H16 0.9500 . ?
C16 C17 1.384(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(4) . ?
C18 H18 0.9500 . ?

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
C13 Te1 Cr1 103.71(7) . . ?
N1 Cr1 Te1 101.86(6) . . ?
N2 Cr1 Te1 107.35(8) . . ?
N2 Cr1 N1 107.24(10) . . ?
N2 Cr1 N3 105.42(10) . . ?
N3 Cr1 Te1 112.82(6) . . ?
N3 Cr1 N1 121.42(8) . . ?
C1 N1 Cr1 127.73(15) . . ?
C1 N1 C4 114.40(18) . . ?
C4 N1 Cr1 117.85(15) . . ?
C7 N3 Cr1 114.39(15) . . ?
C10 N3 Cr1 130.88(15) . . ?
C10 N3 C7 114.50(18) . . ?
N1 C1 H1 107.7 . . ?
N1 C1 C2 110.6(2) . . ?
N1 C1 C3 111.1(2) . . ?
C2 C1 H1 107.7 . . ?
C3 C1 H1 107.7 . . ?
C3 C1 C2 111.8(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4 106.9 . . ?
N1 C4 C5 113.1(2) . . ?
N1 C4 C6 110.91(19) . . ?
C5 C4 H4 106.9 . . ?
C5 C4 C6 111.7(2) . . ?
C6 C4 H4 106.9 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N3 C7 H7 106.8 . . ?
N3 C7 C8 112.8(2) . . ?
N3 C7 C9 110.3(2) . . ?
C8 C7 H7 106.8 . . ?
C9 C7 H7 106.8 . . ?
C9 C7 C8 112.9(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C10 H10 107.6 . . ?
N3 C10 C11 111.2(2) . . ?
N3 C10 C12 111.7(2) . . ?
C11 C10 H10 107.6 . . ?
C11 C10 C12 111.0(2) . . ?
C12 C10 H10 107.6 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C14 C13 Te1 118.48(19) . . ?
C18 C13 Te1 122.74(18) . . ?
C18 C13 C14 118.7(2) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 C13 120.4(3) . . ?
C15 C14 H14 119.8 . . ?
C14 C15 H15 119.5 . . ?
C16 C15 C14 121.0(3) . . ?
C16 C15 H15 119.5 . . ?
C15 C16 H16 120.5 . . ?
C15 C16 C17 119.1(3) . . ?
C17 C16 H16 120.5 . . ?
C16 C17 H17 119.8 . . ?
C16 C17 C18 120.4(3) . . ?
C18 C17 H17 119.8 . . ?
C13 C18 C17 120.5(2) . . ?
C13 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?

# start Validation Reply Form
_vrf_PLAT073_rbd-1-127c          
;
PROBLEM: H-atoms ref, but _hydrogen_treatment reported as     constr       
RESPONSE: Olex2 was used to refine this structure, which provides e.s.d.s
for rider atoms, causing this spurious checkCIF alert
;
_database_code_depnum_ccdc_archive 'CCDC 1000433'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
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#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_aks_crseph_0m
_audit_creation_date             2014-02-24
_audit_creation_method           
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C18 H33 Cr N3 Se'
_chemical_formula_sum            'C18 H33 Cr N3 Se'
_chemical_formula_weight         422.43
_chemical_melting_point          ?
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'
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'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   7.6213(6)
_cell_length_b                   14.7207(11)
_cell_length_c                   18.6479(14)
_cell_angle_alpha                90
_cell_angle_beta                 90.9310(10)
_cell_angle_gamma                90
_cell_volume                     2091.8(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9818
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.404
_cell_measurement_theta_min      2.184
_shelx_estimated_absorpt_T_max   0.774
_shelx_estimated_absorpt_T_min   0.630
_exptl_absorpt_coefficient_mu    2.290
_exptl_absorpt_correction_T_max  0.8877
_exptl_absorpt_correction_T_min  0.7734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0580 before and 0.0518 after correction.
The Ratio of minimum to maximum transmission is 0.8712.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_modifier   ?
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.118
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51088
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.403
_diffrn_reflns_theta_min         1.763
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3330
_reflns_number_total             3846
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material  
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_data_collection       cosmo
_computing_structure_solution    shelxT
_refine_diff_density_max         1.496
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.073
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         3846
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0354
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+3.7657P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0853
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C9(H9), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C18(H18), C19(H19), C20(H20), C21(H21)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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
Se1 Se 0.41379(4) 0.23052(2) 0.29117(2) 0.03032(11) Uani 1 1 d . . . . .
Cr1 Cr 0.44275(6) 0.17014(3) 0.17272(2) 0.01992(12) Uani 1 1 d . . . . .
N3 N 0.4379(3) 0.04660(16) 0.17180(12) 0.0209(5) Uani 1 1 d . . . . .
C2 C 0.5887(4) -0.0164(2) 0.16470(18) 0.0287(7) Uani 1 1 d . . . . .
H2 H 0.5421 -0.0798 0.1668 0.034 Uiso 1 1 calc R . . . .
C3 C 0.6771(5) -0.0047(3) 0.09293(19) 0.0388(8) Uani 1 1 d . . . . .
H3A H 0.5892 -0.0099 0.0542 0.058 Uiso 1 1 calc GR . . . .
H3B H 0.7665 -0.0519 0.0873 0.058 Uiso 1 1 calc GR . . . .
H3C H 0.7325 0.0553 0.0910 0.058 Uiso 1 1 calc GR . . . .
C4 C 0.7180(5) -0.0046(3) 0.2266(2) 0.0443(9) Uani 1 1 d . . . . .
H4A H 0.7768 0.0544 0.2224 0.067 Uiso 1 1 calc GR . . . .
H4B H 0.8056 -0.0532 0.2254 0.067 Uiso 1 1 calc GR . . . .
H4C H 0.6553 -0.0072 0.2720 0.067 Uiso 1 1 calc GR . . . .
C5 C 0.2655(4) 0.0010(2) 0.17491(16) 0.0251(6) Uani 1 1 d . . . . .
H5 H 0.1747 0.0496 0.1796 0.030 Uiso 1 1 calc R . . . .
C6 C 0.2210(4) -0.0522(2) 0.10675(18) 0.0356(8) Uani 1 1 d . . . . .
H6A H 0.2365 -0.0129 0.0649 0.053 Uiso 1 1 calc GR . . . .
H6B H 0.0989 -0.0729 0.1083 0.053 Uiso 1 1 calc GR . . . .
H6C H 0.2991 -0.1049 0.1033 0.053 Uiso 1 1 calc GR . . . .
C7 C 0.2529(5) -0.0596(2) 0.24093(18) 0.0347(8) Uani 1 1 d . . . . .
H7A H 0.3288 -0.1128 0.2352 0.052 Uiso 1 1 calc GR . . . .
H7B H 0.1312 -0.0796 0.2465 0.052 Uiso 1 1 calc GR . . . .
H7C H 0.2906 -0.0254 0.2836 0.052 Uiso 1 1 calc GR . . . .
N2 N 0.3205(3) 0.23467(16) 0.10501(12) 0.0203(5) Uani 1 1 d . . . . .
C9 C 0.1269(4) 0.2280(2) 0.10793(17) 0.0258(7) Uani 1 1 d . . . . .
H9 H 0.0984 0.1875 0.1492 0.031 Uiso 1 1 calc R . . . .
C10 C 0.0448(4) 0.3203(2) 0.1227(2) 0.0351(8) Uani 1 1 d . . . . .
H10A H 0.1052 0.3487 0.1638 0.053 Uiso 1 1 calc GR . . . .
H10B H -0.0796 0.3124 0.1336 0.053 Uiso 1 1 calc GR . . . .
H10C H 0.0561 0.3591 0.0804 0.053 Uiso 1 1 calc GR . . . .
C11 C 0.0473(4) 0.1846(2) 0.04055(19) 0.0385(8) Uani 1 1 d . . . . .
H11A H 0.0713 0.2231 -0.0010 0.058 Uiso 1 1 calc GR . . . .
H11B H -0.0798 0.1784 0.0460 0.058 Uiso 1 1 calc GR . . . .
H11C H 0.0994 0.1245 0.0334 0.058 Uiso 1 1 calc GR . . . .
C12 C 0.3885(4) 0.2918(2) 0.04675(16) 0.0261(7) Uani 1 1 d . . . . .
H12 H 0.2855 0.3138 0.0178 0.031 Uiso 1 1 calc R . . . .
C13 C 0.4842(5) 0.3750(2) 0.0762(2) 0.0394(8) Uani 1 1 d . . . . .
H13A H 0.4057 0.4092 0.1073 0.059 Uiso 1 1 calc GR . . . .
H13B H 0.5206 0.4136 0.0363 0.059 Uiso 1 1 calc GR . . . .
H13C H 0.5880 0.3556 0.1039 0.059 Uiso 1 1 calc GR . . . .
C14 C 0.5038(5) 0.2373(2) -0.00272(18) 0.0367(8) Uani 1 1 d . . . . .
H14A H 0.6068 0.2151 0.0241 0.055 Uiso 1 1 calc GR . . . .
H14B H 0.5420 0.2759 -0.0423 0.055 Uiso 1 1 calc GR . . . .
H14C H 0.4373 0.1855 -0.0220 0.055 Uiso 1 1 calc GR . . . .
N1 N 0.6356(3) 0.19668(17) 0.16143(14) 0.0274(6) Uani 1 1 d . . . . .
C16 C 0.2092(4) 0.1751(2) 0.33128(16) 0.0261(7) Uani 1 1 d . . . . .
C17 C 0.2309(5) 0.1049(2) 0.38050(17) 0.0334(7) Uani 1 1 d . . . . .
H17 H 0.3453 0.0826 0.3912 0.040 Uiso 1 1 calc R . . . .
C18 C 0.0882(6) 0.0674(3) 0.4139(2) 0.0497(10) Uani 1 1 d . . . . .
H18 H 0.1046 0.0194 0.4474 0.060 Uiso 1 1 calc R . . . .
C19 C -0.0764(6) 0.0991(4) 0.3989(2) 0.0635(14) Uani 1 1 d . . . . .
H19 H -0.1747 0.0732 0.4220 0.076 Uiso 1 1 calc R . . . .
C20 C -0.1001(5) 0.1683(4) 0.3506(3) 0.0643(14) Uani 1 1 d . . . . .
H20 H -0.2152 0.1899 0.3402 0.077 Uiso 1 1 calc R . . . .
C21 C 0.0431(5) 0.2074(3) 0.3165(2) 0.0432(9) Uani 1 1 d . . . . .
H21 H 0.0260 0.2558 0.2835 0.052 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Se1 Cr1 2.3945(6) . ?
Se1 C16 1.922(3) . ?
Cr1 N3 1.819(2) . ?
Cr1 N2 1.824(2) . ?
Cr1 N1 1.539(3) . ?
N3 C2 1.484(4) . ?
N3 C5 1.478(4) . ?
C2 H2 1.0000 . ?
C2 C3 1.518(5) . ?
C2 C4 1.515(5) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 H5 1.0000 . ?
C5 C6 1.526(4) . ?
C5 C7 1.524(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
N2 C9 1.481(4) . ?
N2 C12 1.474(4) . ?
C9 H9 1.0000 . ?
C9 C10 1.523(4) . ?
C9 C11 1.526(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12 1.0000 . ?
C12 C13 1.524(5) . ?
C12 C14 1.515(4) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C16 C17 1.390(4) . ?
C16 C21 1.375(5) . ?
C17 H17 0.9500 . ?
C17 C18 1.377(5) . ?
C18 H18 0.9500 . ?
C18 C19 1.363(7) . ?
C19 H19 0.9500 . ?
C19 C20 1.370(7) . ?
C20 H20 0.9500 . ?
C20 C21 1.396(6) . ?
C21 H21 0.9500 . ?

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
C16 Se1 Cr1 106.80(9) . . ?
N3 Cr1 Se1 112.19(8) . . ?
N3 Cr1 N2 120.28(11) . . ?
N2 Cr1 Se1 113.05(8) . . ?
N1 Cr1 Se1 97.73(10) . . ?
N1 Cr1 N3 105.78(12) . . ?
N1 Cr1 N2 104.56(12) . . ?
C2 N3 Cr1 127.58(19) . . ?
C5 N3 Cr1 118.16(18) . . ?
C5 N3 C2 114.2(2) . . ?
N3 C2 H2 107.7 . . ?
N3 C2 C3 111.3(3) . . ?
N3 C2 C4 110.8(3) . . ?
C3 C2 H2 107.7 . . ?
C4 C2 H2 107.7 . . ?
C4 C2 C3 111.5(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N3 C5 H5 107.2 . . ?
N3 C5 C6 112.7(2) . . ?
N3 C5 C7 111.4(3) . . ?
C6 C5 H5 107.2 . . ?
C7 C5 H5 107.2 . . ?
C7 C5 C6 110.9(3) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 N2 Cr1 115.98(18) . . ?
C12 N2 Cr1 128.71(19) . . ?
C12 N2 C9 115.3(2) . . ?
N2 C9 H9 107.3 . . ?
N2 C9 C10 111.1(2) . . ?
N2 C9 C11 112.4(3) . . ?
C10 C9 H9 107.3 . . ?
C10 C9 C11 111.3(3) . . ?
C11 C9 H9 107.3 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12 107.5 . . ?
N2 C12 C13 111.4(3) . . ?
N2 C12 C14 111.2(2) . . ?
C13 C12 H12 107.5 . . ?
C14 C12 H12 107.5 . . ?
C14 C12 C13 111.5(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C17 C16 Se1 118.9(2) . . ?
C21 C16 Se1 121.7(3) . . ?
C21 C16 C17 119.2(3) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 C16 120.7(4) . . ?
C18 C17 H17 119.6 . . ?
C17 C18 H18 120.0 . . ?
C19 C18 C17 120.0(4) . . ?
C19 C18 H18 120.0 . . ?
C18 C19 H19 120.0 . . ?
C18 C19 C20 120.0(4) . . ?
C20 C19 H19 120.0 . . ?
C19 C20 H20 119.7 . . ?
C19 C20 C21 120.7(4) . . ?
C21 C20 H20 119.7 . . ?
C16 C21 C20 119.4(4) . . ?
C16 C21 H21 120.3 . . ?
C20 C21 H21 120.3 . . ?

_database_code_depnum_ccdc_archive 'CCDC 1000434'
