#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:13:40 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295281 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/65/7716554.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7716554
loop_
_publ_author_name
'Chong, Julien'
'Benchohra, Amina'
'Besnard, Céline'
'Guénée, Laure'
'Rosspeintner, Arnulf'
'Cruz, Carlos M.'
'Jiménez, Juan-Ramón'
'Piguet, Claude'
_publ_section_title
;
 Taming 2,2'-biimidazole ligands in trivalent chromium complexes.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15801
_journal_page_last               15814
_journal_paper_doi               10.1039/d4dt01608d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H20 Cl2 Cr N8, Cl, 3(C H4 O)'
_chemical_formula_sum            'C19 H32 Cl3 Cr N8 O3'
_chemical_formula_weight         578.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-02-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-15 deposited with the CCDC.	2024-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                99.106(2)
_cell_angle_beta                 95.598(2)
_cell_angle_gamma                104.370(2)
_cell_formula_units_Z            2
_cell_length_a                   6.8363(2)
_cell_length_b                   13.7717(3)
_cell_length_c                   14.7817(3)
_cell_measurement_reflns_used    7172
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      72.5010
_cell_measurement_theta_min      3.3810
_cell_volume                     1317.44(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00 -58.00   0.50   10.00    --  -57.33   0.00 -30.00   52
  2  ω   -101.00 -75.00   0.50   10.00    --  -57.33 -15.00 150.00   52
  3  ω    -55.00 -19.00   0.50   10.00    --  -57.33   0.00 -30.00   72
  4  ω     22.00  47.00   0.50   10.00    --   60.24 -94.00  30.00   50
  5  ω     27.00  77.00   0.50   10.00    --   60.24  15.00 150.00  100
  6  ω     21.00  66.00   0.50   10.00    --   60.24 -94.00 -60.00   90
  7  ω     22.00  70.00   0.50   10.00    --   60.24 -94.00 -90.00   96
  8  ω     45.00  85.00   0.50   10.00    --   60.24-125.00-180.00   80
  9  ω     40.00  70.00   0.50   10.00    --   60.24 -94.00  60.00   60
 10  ω     26.00  59.00   0.50   10.00    --   60.24 -94.00 -30.00   66
 11  ω     36.00  89.00   0.50   10.00    --   60.24-125.00-120.00  106
 12  ω     47.00 118.00   0.50   10.00    --   74.64  15.00-180.00  142
 13  ω     58.00  84.00   0.50   10.00    --   74.64 -94.00  30.00   52
 14  ω     41.00 119.00   0.50   10.00    --   74.64  15.00  30.00  156
 15  ω     45.00  81.00   0.50   10.00    --   79.80 -94.00-150.00   72
 16  ω     57.00 120.00   0.50   10.00    --   79.80  15.00 120.00  126
 17  ω     43.00  96.00   0.50   10.00    --   79.80-107.00 -16.00  106
 18  ω     51.00 102.00   0.50   10.00    --   79.80-125.00 -60.00  102
 19  ω     40.00  74.00   0.50   10.00    --   79.80   0.00 120.00   68
 20  ω     44.00  69.00   0.50   10.00    --   79.80 -94.00  30.00   50
 21  ω     73.00 105.00   0.50   10.00    --   79.80-125.00 -90.00   64
 22  ω     59.00 108.00   0.50   10.00    --   79.80-125.00  90.00   98
 23  ω     43.00  70.00   0.50   10.00    --   79.80-125.00 -90.00   54
 24  ω     44.00  72.00   0.50   10.00    --   79.80 -94.00 150.00   56
 25  ω     47.00  76.00   0.50   10.00    --   79.80-125.00 120.00   58
 26  ω     61.00 108.00   0.50   10.00    --   79.80-125.00-150.00   94
 27  ω     41.00  90.00   0.50   10.00    --   79.80 -94.00 120.00   98
 28  ω     50.00 124.00   0.50   10.00    --   79.80  15.00 -30.00  148
 29  ω     61.00  87.00   0.50   10.00    --   79.80 -94.00  60.00   52
 30  ω     46.00  88.00   0.50   10.00    --   79.80 -94.00   0.00   84
 31  ω     40.00  80.00   0.50   10.00    --   79.80 -94.00 -60.00   80
 32  ω     83.00 108.00   0.50   10.00    --   79.80-125.00 120.00   50
 33  ω    104.00 131.00   0.50   10.00    --   83.50  18.00-114.25   54
 34  ω     53.00  83.00   0.50   10.00    --   83.50  18.00-114.25   60
 35  ω     49.00 127.00   0.50   10.00    --   83.50  17.00-178.39  156
 36  ω     60.00 106.00   0.50   10.00    --   83.50  16.00  63.19   92
 37  ω     98.00 123.00   0.50   10.00    --   83.50 152.00 -66.90   50
 38  ω     97.00 122.00   0.50   10.00    --   83.50-139.00  32.80   50
 39  ω     44.00  74.00   0.50   10.00    --   83.50-139.00  32.80   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0077072000
_diffrn_orient_matrix_UB_12      -0.0800474000
_diffrn_orient_matrix_UB_13      -0.0867636000
_diffrn_orient_matrix_UB_21      0.0508045000
_diffrn_orient_matrix_UB_22      0.0854887000
_diffrn_orient_matrix_UB_23      -0.0566361000
_diffrn_orient_matrix_UB_31      0.2293593000
_diffrn_orient_matrix_UB_32      0.0107053000
_diffrn_orient_matrix_UB_33      0.0252646000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0618
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17103
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.776
_diffrn_reflns_theta_min         3.059
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.686
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.531
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       needle
_exptl_crystal_F_000             602
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         5256
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0704
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1191P)²+1.3207P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1859
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4337
_reflns_number_total             5256
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_database_code               7716554
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 H32 Cl3 Cr N8 O3'
_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.
;
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.334
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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, All O(H) groups, All O(H,H) groups
2. Others
 Sof(H3BB)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(H19C)=1-FVAR(1)
 Sof(H3AA)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15)
3.b Tetrahedral OH refined with riding coordinates:
 O3(H3BB), O3(H3AA)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C19A(H19D,H19E,
 H19F)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A), O2(H2A)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.614
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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 0.77773(9) 0.79905(5) 0.62531(4) 0.0237(2) Uani 1 1 d . . . . .
Cl1 Cl 1.00104(15) 0.70039(8) 0.65030(8) 0.0336(3) Uani 1 1 d . . . . .
Cl2 Cl 0.87757(15) 0.82184(8) 0.48181(7) 0.0294(2) Uani 1 1 d . . . . .
N1 N 0.6563(5) 0.7665(3) 0.7402(3) 0.0309(8) Uani 1 1 d . . . . .
N2 N 0.4358(6) 0.6718(3) 0.8104(3) 0.0354(8) Uani 1 1 d . . . . .
N3 N 0.5303(5) 0.6774(2) 0.5705(2) 0.0267(7) Uani 1 1 d . . . . .
N4 N 0.2941(5) 0.5429(3) 0.5882(3) 0.0291(8) Uani 1 1 d . . . . .
N5 N 0.6088(5) 0.9016(2) 0.6183(2) 0.0259(7) Uani 1 1 d . . . . .
N6 N 0.5813(5) 1.0587(2) 0.6352(2) 0.0278(7) Uani 1 1 d . . . . .
N7 N 0.9727(5) 0.9303(3) 0.7003(2) 0.0270(7) Uani 1 1 d . . . . .
N8 N 1.0546(6) 1.0951(3) 0.7533(2) 0.0320(8) Uani 1 1 d . . . . .
C1 C 0.6901(8) 0.8100(4) 0.8311(3) 0.0415(11) Uani 1 1 d . . . . .
H1 H 0.791154 0.871078 0.859168 0.050 Uiso 1 1 calc R U . . .
C2 C 0.5554(8) 0.7517(4) 0.8753(3) 0.0436(11) Uani 1 1 d . . . . .
H2 H 0.545941 0.764064 0.939622 0.052 Uiso 1 1 calc R U . . .
C3 C 0.2653(8) 0.5949(4) 0.8337(4) 0.0499(13) Uani 1 1 d . . . . .
H3A H 0.253763 0.612499 0.899450 0.075 Uiso 1 1 calc R U . . .
H3B H 0.290988 0.527450 0.820861 0.075 Uiso 1 1 calc R U . . .
H3C H 0.137992 0.593608 0.796170 0.075 Uiso 1 1 calc R U . . .
C4 C 0.4991(6) 0.6828(3) 0.7287(3) 0.0292(9) Uani 1 1 d . . . . .
C5 C 0.4348(6) 0.6292(3) 0.6329(3) 0.0281(8) Uani 1 1 d . . . . .
C6 C 0.4437(6) 0.6223(3) 0.4847(3) 0.0294(9) Uani 1 1 d . . . . .
H6 H 0.479079 0.639123 0.427432 0.035 Uiso 1 1 calc R U . . .
C7 C 0.2981(6) 0.5394(3) 0.4953(3) 0.0305(9) Uani 1 1 d . . . . .
H7 H 0.213840 0.488011 0.446836 0.037 Uiso 1 1 calc R U . . .
C8 C 0.1662(7) 0.4615(3) 0.6267(4) 0.0385(10) Uani 1 1 d . . . . .
H8A H 0.060591 0.486683 0.655498 0.058 Uiso 1 1 calc R U . . .
H8B H 0.251003 0.440645 0.673264 0.058 Uiso 1 1 calc R U . . .
H8C H 0.101566 0.402835 0.576900 0.058 Uiso 1 1 calc R U . . .
C9 C 0.4166(6) 0.8982(3) 0.5804(3) 0.0248(8) Uani 1 1 d . . . . .
H9 H 0.312991 0.838237 0.551849 0.030 Uiso 1 1 calc R U . . .
C10 C 0.3986(6) 0.9950(3) 0.5905(3) 0.0274(8) Uani 1 1 d . . . . .
H10 H 0.280919 1.014994 0.570260 0.033 Uiso 1 1 calc R U . . .
C11 C 0.6203(8) 1.1698(3) 0.6556(3) 0.0378(10) Uani 1 1 d . . . . .
H11A H 0.737903 1.200869 0.627101 0.057 Uiso 1 1 calc R U . . .
H11B H 0.649120 1.193964 0.722826 0.057 Uiso 1 1 calc R U . . .
H11C H 0.500036 1.188901 0.630723 0.057 Uiso 1 1 calc R U . . .
C12 C 0.7072(6) 0.9995(3) 0.6524(3) 0.0256(8) Uani 1 1 d . . . . .
C13 C 0.9126(6) 1.0156(3) 0.7003(3) 0.0266(8) Uani 1 1 d . . . . .
C14 C 1.1578(6) 0.9561(4) 0.7558(3) 0.0322(9) Uani 1 1 d . . . . .
H14 H 1.236443 0.910661 0.768676 0.039 Uiso 1 1 calc R U . . .
C15 C 1.2084(7) 1.0578(4) 0.7889(3) 0.0372(10) Uani 1 1 d . . . . .
H15 H 1.328453 1.096411 0.829456 0.045 Uiso 1 1 calc R U . . .
C16 C 1.0613(8) 1.2040(3) 0.7738(4) 0.0427(11) Uani 1 1 d . . . . .
H16A H 1.062193 1.230981 0.716337 0.064 Uiso 1 1 calc R U . . .
H16B H 1.185091 1.241423 0.816805 0.064 Uiso 1 1 calc R U . . .
H16C H 0.941038 1.212159 0.802062 0.064 Uiso 1 1 calc R U . . .
Cl3 Cl 0.61515(19) 0.27670(10) 0.90550(8) 0.0453(3) Uani 1 1 d . . . . .
O1 O 0.5242(6) 0.4007(3) 0.7523(3) 0.0629(11) Uani 1 1 d . . . . .
H1A H 0.521167 0.370193 0.797244 0.094 Uiso 1 1 calc R U . . .
C17 C 0.7030(9) 0.4704(5) 0.7618(4) 0.0612(16) Uani 1 1 d . . . . .
H17A H 0.813918 0.437610 0.768986 0.092 Uiso 1 1 calc R U . . .
H17B H 0.715189 0.523037 0.816679 0.092 Uiso 1 1 calc R U . . .
H17C H 0.711210 0.501873 0.706806 0.092 Uiso 1 1 calc R U . . .
O2 O 1.0573(8) 0.4063(4) 0.8991(4) 0.0833(15) Uani 1 1 d . . . . .
H2A H 0.935566 0.377523 0.902987 0.125 Uiso 1 1 calc R U . . .
C18 C 1.1840(12) 0.4081(6) 0.9820(5) 0.078(2) Uani 1 1 d . . . . .
H18A H 1.118073 0.352529 1.012035 0.118 Uiso 1 1 calc R U . . .
H18B H 1.205206 0.473640 1.023975 0.118 Uiso 1 1 calc R U . . .
H18C H 1.315908 0.399322 0.967201 0.118 Uiso 1 1 calc R U . . .
O3 O 0.7279(10) 0.0696(4) 0.9013(4) 0.0951(18) Uani 1 1 d . . . . .
H3BB H 0.698761 0.124449 0.896102 0.143 Uiso 0.48(5) 1 calc R U P A 2
H3AA H 0.687559 0.121590 0.896041 0.143 Uiso 0.52(5) 1 calc R U P A 1
C19B C 0.709(9) 0.051(3) 0.9966(19) 0.143(14) Uani 0.48(5) 1 d . . P A 2
H19A H 0.744927 0.115828 1.040191 0.215 Uiso 0.48(5) 1 calc R U P A 2
H19B H 0.802146 0.010114 1.013188 0.215 Uiso 0.48(5) 1 calc R U P A 2
H19C H 0.568704 0.013033 0.999333 0.215 Uiso 0.48(5) 1 calc R U P A 2
C19A C 0.848(7) 0.087(2) 0.9791(19) 0.112(14) Uani 0.52(5) 1 d . . P A 1
H19D H 0.973305 0.139352 0.977341 0.168 Uiso 0.52(5) 1 calc R U P A 1
H19E H 0.881284 0.023939 0.988842 0.168 Uiso 0.52(5) 1 calc R U P A 1
H19F H 0.779031 0.110932 1.029930 0.168 Uiso 0.52(5) 1 calc R U P A 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -1 -5 0.0040
-1 1 5 0.0090
4 -2 1 0.0975
-4 2 -1 0.0975
0 5 -3 0.0126
0 -5 3 0.0076
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
Cl1 Cr1 Cl2 92.54(4) . . ?
N1 Cr1 Cl1 89.68(11) . . ?
N1 Cr1 Cl2 172.38(11) . . ?
N1 Cr1 N3 78.17(14) . . ?
N1 Cr1 N5 88.51(14) . . ?
N1 Cr1 N7 90.74(14) . . ?
N3 Cr1 Cl1 95.24(10) . . ?
N3 Cr1 Cl2 94.36(10) . . ?
N5 Cr1 Cl1 171.68(10) . . ?
N5 Cr1 Cl2 90.31(10) . . ?
N5 Cr1 N3 92.33(13) . . ?
N7 Cr1 Cl1 93.99(10) . . ?
N7 Cr1 Cl2 96.38(10) . . ?
N7 Cr1 N3 165.50(14) . . ?
N7 Cr1 N5 77.92(14) . . ?
C1 N1 Cr1 136.1(3) . . ?
C4 N1 Cr1 116.8(3) . . ?
C4 N1 C1 107.1(4) . . ?
C2 N2 C3 122.1(4) . . ?
C4 N2 C2 107.3(4) . . ?
C4 N2 C3 130.5(4) . . ?
C5 N3 Cr1 115.2(3) . . ?
C5 N3 C6 107.4(3) . . ?
C6 N3 Cr1 136.9(3) . . ?
C5 N4 C7 107.1(3) . . ?
C5 N4 C8 129.3(4) . . ?
C7 N4 C8 123.5(4) . . ?
C9 N5 Cr1 136.0(3) . . ?
C12 N5 Cr1 116.0(3) . . ?
C12 N5 C9 107.8(3) . . ?
C10 N6 C11 122.9(4) . . ?
C12 N6 C10 107.4(3) . . ?
C12 N6 C11 129.7(4) . . ?
C13 N7 Cr1 116.4(3) . . ?
C13 N7 C14 107.6(4) . . ?
C14 N7 Cr1 136.0(3) . . ?
C13 N8 C15 107.3(4) . . ?
C13 N8 C16 130.3(4) . . ?
C15 N8 C16 122.3(4) . . ?
N1 C1 H1 125.7 . . ?
N1 C1 C2 108.5(4) . . ?
C2 C1 H1 125.7 . . ?
N2 C2 H2 126.3 . . ?
C1 C2 N2 107.3(4) . . ?
C1 C2 H2 126.3 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C5 114.4(4) . . ?
N2 C4 N1 109.7(4) . . ?
N2 C4 C5 135.9(4) . . ?
N3 C5 N4 109.4(4) . . ?
N3 C5 C4 114.4(4) . . ?
N4 C5 C4 136.1(4) . . ?
N3 C6 H6 125.9 . . ?
C7 C6 N3 108.2(4) . . ?
C7 C6 H6 125.9 . . ?
N4 C7 H7 126.0 . . ?
C6 C7 N4 107.9(4) . . ?
C6 C7 H7 126.0 . . ?
N4 C8 H8A 109.5 . . ?
N4 C8 H8B 109.5 . . ?
N4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N5 C9 H9 125.9 . . ?
C10 C9 N5 108.3(4) . . ?
C10 C9 H9 125.9 . . ?
N6 C10 H10 126.2 . . ?
C9 C10 N6 107.5(4) . . ?
C9 C10 H10 126.2 . . ?
N6 C11 H11A 109.5 . . ?
N6 C11 H11B 109.5 . . ?
N6 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N5 C12 N6 109.0(3) . . ?
N5 C12 C13 114.5(4) . . ?
N6 C12 C13 136.4(4) . . ?
N7 C13 N8 109.6(4) . . ?
N7 C13 C12 114.4(3) . . ?
N8 C13 C12 135.7(4) . . ?
N7 C14 H14 126.1 . . ?
C15 C14 N7 107.9(4) . . ?
C15 C14 H14 126.1 . . ?
N8 C15 H15 126.2 . . ?
C14 C15 N8 107.6(4) . . ?
C14 C15 H15 126.2 . . ?
N8 C16 H16A 109.5 . . ?
N8 C16 H16B 109.5 . . ?
N8 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C17 O1 H1A 109.5 . . ?
O1 C17 H17A 109.5 . . ?
O1 C17 H17B 109.5 . . ?
O1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 O2 H2A 109.5 . . ?
O2 C18 H18A 109.5 . . ?
O2 C18 H18B 109.5 . . ?
O2 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C19B O3 H3BB 109.5 . . ?
C19A O3 H3AA 109.5 . . ?
O3 C19B H19A 109.5 . . ?
O3 C19B H19B 109.5 . . ?
O3 C19B H19C 109.5 . . ?
H19A C19B H19B 109.5 . . ?
H19A C19B H19C 109.5 . . ?
H19B C19B H19C 109.5 . . ?
O3 C19A H19D 109.5 . . ?
O3 C19A H19E 109.5 . . ?
O3 C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
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 Cl1 2.3219(11) . ?
Cr1 Cl2 2.3346(11) . ?
Cr1 N1 2.025(4) . ?
Cr1 N3 2.054(3) . ?
Cr1 N5 2.043(3) . ?
Cr1 N7 2.038(3) . ?
N1 C1 1.355(6) . ?
N1 C4 1.342(5) . ?
N2 C2 1.367(6) . ?
N2 C3 1.476(6) . ?
N2 C4 1.340(6) . ?
N3 C5 1.348(5) . ?
N3 C6 1.364(5) . ?
N4 C5 1.354(5) . ?
N4 C7 1.370(6) . ?
N4 C8 1.468(5) . ?
N5 C9 1.364(5) . ?
N5 C12 1.339(5) . ?
N6 C10 1.370(5) . ?
N6 C11 1.462(5) . ?
N6 C12 1.357(5) . ?
N7 C13 1.337(5) . ?
N7 C14 1.373(5) . ?
N8 C13 1.344(5) . ?
N8 C15 1.376(6) . ?
N8 C16 1.471(6) . ?
C1 H1 0.9500 . ?
C1 C2 1.355(7) . ?
C2 H2 0.9500 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C5 1.458(6) . ?
C6 H6 0.9500 . ?
C6 C7 1.357(6) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9 0.9500 . ?
C9 C10 1.355(5) . ?
C10 H10 0.9500 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.457(6) . ?
C14 H14 0.9500 . ?
C14 C15 1.352(7) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
O1 H1A 0.8400 . ?
O1 C17 1.333(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
O2 H2A 0.8400 . ?
O2 C18 1.424(9) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
O3 H3BB 0.8400 . ?
O3 H3AA 0.8400 . ?
O3 C19B 1.49(2) . ?
O3 C19A 1.297(18) . ?
C19B H19A 0.9800 . ?
C19B H19B 0.9800 . ?
C19B H19C 0.9800 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
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
_geom_hbond_publ_flag
O1 H1A Cl3 0.84 2.34 3.148(4) 160.4 . yes
O2 H2A Cl3 0.84 2.29 3.124(5) 171.5 . yes
O3 H3BB Cl3 0.84 2.29 3.126(6) 171.3 . yes
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
Cr1 N1 C1 C2 179.5(4) . . . . ?
Cr1 N1 C4 N2 -179.9(3) . . . . ?
Cr1 N1 C4 C5 -2.0(5) . . . . ?
Cr1 N3 C5 N4 -171.5(2) . . . . ?
Cr1 N3 C5 C4 11.0(4) . . . . ?
Cr1 N3 C6 C7 170.2(3) . . . . ?
Cr1 N5 C9 C10 -173.5(3) . . . . ?
Cr1 N5 C12 N6 174.5(2) . . . . ?
Cr1 N5 C12 C13 -7.7(4) . . . . ?
Cr1 N7 C13 N8 179.2(2) . . . . ?
Cr1 N7 C13 C12 4.9(4) . . . . ?
Cr1 N7 C14 C15 -178.3(3) . . . . ?
N1 C1 C2 N2 -0.6(6) . . . . ?
N1 C4 C5 N3 -6.0(5) . . . . ?
N1 C4 C5 N4 177.4(4) . . . . ?
N2 C4 C5 N3 171.2(5) . . . . ?
N2 C4 C5 N4 -5.4(9) . . . . ?
N3 C6 C7 N4 0.0(5) . . . . ?
N5 C9 C10 N6 -0.2(5) . . . . ?
N5 C12 C13 N7 1.9(5) . . . . ?
N5 C12 C13 N8 -170.4(4) . . . . ?
N6 C12 C13 N7 178.8(4) . . . . ?
N6 C12 C13 N8 6.5(8) . . . . ?
N7 C14 C15 N8 -0.4(5) . . . . ?
C1 N1 C4 N2 -1.0(5) . . . . ?
C1 N1 C4 C5 176.9(4) . . . . ?
C2 N2 C4 N1 0.7(5) . . . . ?
C2 N2 C4 C5 -176.6(5) . . . . ?
C3 N2 C2 C1 -177.2(5) . . . . ?
C3 N2 C4 N1 177.6(5) . . . . ?
C3 N2 C4 C5 0.3(9) . . . . ?
C4 N1 C1 C2 1.0(6) . . . . ?
C4 N2 C2 C1 0.0(6) . . . . ?
C5 N3 C6 C7 -1.2(4) . . . . ?
C5 N4 C7 C6 1.2(4) . . . . ?
C6 N3 C5 N4 2.0(4) . . . . ?
C6 N3 C5 C4 -175.5(3) . . . . ?
C7 N4 C5 N3 -2.0(4) . . . . ?
C7 N4 C5 C4 174.7(4) . . . . ?
C8 N4 C5 N3 174.1(4) . . . . ?
C8 N4 C5 C4 -9.2(8) . . . . ?
C8 N4 C7 C6 -175.1(4) . . . . ?
C9 N5 C12 N6 -1.1(4) . . . . ?
C9 N5 C12 C13 176.6(3) . . . . ?
C10 N6 C12 N5 1.0(4) . . . . ?
C10 N6 C12 C13 -176.0(4) . . . . ?
C11 N6 C10 C9 178.2(4) . . . . ?
C11 N6 C12 N5 -177.5(4) . . . . ?
C11 N6 C12 C13 5.4(8) . . . . ?
C12 N5 C9 C10 0.8(4) . . . . ?
C12 N6 C10 C9 -0.5(4) . . . . ?
C13 N7 C14 C15 -0.2(5) . . . . ?
C13 N8 C15 C14 0.8(5) . . . . ?
C14 N7 C13 N8 0.7(4) . . . . ?
C14 N7 C13 C12 -173.6(3) . . . . ?
C15 N8 C13 N7 -0.9(4) . . . . ?
C15 N8 C13 C12 171.7(5) . . . . ?
C16 N8 C13 N7 178.8(4) . . . . ?
C16 N8 C13 C12 -8.7(8) . . . . ?
C16 N8 C15 C14 -178.9(4) . . . . ?
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0011 -1.0044 -4.9975 0.5063 0.2480 0.0926
-1.0011 1.0044 4.9975 -0.5063 -0.2480 -0.0926
3.9985 -1.9981 1.0111 0.0414 -0.0249 0.9213
-3.9985 1.9981 -1.0111 -0.0414 0.0249 -0.9213
-0.0021 4.9952 -2.9997 -0.1396 0.5968 -0.0228
0.0021 -4.9952 2.9997 0.1396 -0.5968 0.0228
