#------------------------------------------------------------------------------
#$Date: 2024-10-06 11:13:40 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295281 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/65/7716552.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_7716552
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         'C30 H20 Cr N8, C F3 O3 S, 1.5(C H4 O)'
_chemical_formula_sum            'C32.5 H26 Cr F3 N8 O4.5 S'
_chemical_formula_weight         741.67
_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             2024-01-17
_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                107.378(3)
_cell_angle_beta                 98.544(3)
_cell_angle_gamma                96.353(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7735(4)
_cell_length_b                   11.8329(4)
_cell_length_c                   12.6821(4)
_cell_measurement_reflns_used    8352
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      70.6220
_cell_measurement_theta_min      3.8270
_cell_volume                     1644.79(10)
_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 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4670
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -79.00 -53.00   1.00    1.00    --  -41.71 125.00 120.00   26
  2  ω    -64.00  26.00   1.00    1.00    --  -41.71  57.00  60.00   90
  3  ω    -62.00  30.00   1.00    1.00    --  -41.71  38.00-150.00   92
  4  ω   -113.00 -19.00   1.00    1.00    --  -41.71 -57.00 -90.00   94
  5  ω     28.00 126.00   1.00    4.00    --  100.00 -45.00 150.00   98
  6  ω     37.00  79.00   1.00    4.00    --  100.00-125.00-150.00   42
  7  ω     38.00  98.00   1.00    4.00    --  100.00 -77.00  30.00   60
  8  ω     75.00 107.00   1.00    4.00    --  100.00 -94.00 -30.00   32
  9  ω     59.00 129.00   1.00    4.00    --  100.00 -61.00-120.00   70
 10  ω     28.00  71.00   1.00    4.00    --  100.00 -45.00  60.00   43
 11  ω    110.00 162.00   1.00    4.00    --  100.00  77.00-180.00   52
 12  ω     49.00  75.00   1.00    4.00    --  100.00 -30.00 -60.00   26
 13  ω    100.00 127.00   1.00    4.00    --  100.00 -30.00 -60.00   27
 14  ω     23.00 106.00   1.00    4.00    --  100.00 -94.00 150.00   83
 15  ω     84.00 111.00   1.00    4.00    --  100.00-125.00  90.00   27
 16  ω     61.00 107.00   1.00    4.00    --  100.00 -94.00-120.00   46
 17  ω     75.00 126.00   1.00    4.00    --  100.00  45.00 -30.00   51
 18  ω     65.00 107.00   1.00    4.00    --  100.00 -94.00 120.00   42
 19  ω     16.00 167.00   1.00    4.00    --  100.00   0.00-180.00  151
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0642480000
_diffrn_orient_matrix_UB_12      -0.0121537000
_diffrn_orient_matrix_UB_13      0.0943806000
_diffrn_orient_matrix_UB_21      -0.0871983000
_diffrn_orient_matrix_UB_22      0.0774212000
_diffrn_orient_matrix_UB_23      -0.0326658000
_diffrn_orient_matrix_UB_31      -0.0791360000
_diffrn_orient_matrix_UB_32      -0.1139512000
_diffrn_orient_matrix_UB_33      -0.0827250000
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12239
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.623
_diffrn_reflns_theta_min         3.721
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.068
_exptl_absorpt_correction_T_max  0.690
_exptl_absorpt_correction_T_min  0.504
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_description       prism
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.616
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0563
_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)+(0.1208P)²+1.2810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5675
_reflns_number_total             6162
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01608d2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7716546--7716554.cif.'
_cod_original_cell_volume        1644.79(9)
_cod_original_formula_sum        'C32.50 H26 Cr F3 N8 O4.50 S'
_cod_database_code               7716552
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32.5 H26 Cr F3 N8 O4.5 S'
_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   0.663
_shelx_estimated_absorpt_t_min   0.395
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_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
2. Others
 Fixed Sof: O4S(0.5) H4S(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C17(H17), C22(H22), C9(H9), C20(H20), C15(H15), C3(H3),
 C5(H5), C30(H30), C29(H29), C8(H8), C1(H1), C21(H21), C25(H25), C14(H14),
 C18(H18), C26(H26), C10(H10), C13(H13)
3.b Idealised Me refined as rotating group:
 C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,H3SC)
3.c Idealised tetrahedral OH refined as rotating group:
 O2S(H2S), O4S(H4S)
;
_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 3.201
_oxdiff_exptl_absorpt_empirical_full_min 0.429
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 0.27914(4) 0.29816(4) 0.66956(3) 0.01938(16) Uani 1 1 d . . . . .
N4 N 0.3605(2) 0.4583(2) 0.7899(2) 0.0246(5) Uani 1 1 d . . . . .
N6 N 0.1082(3) 0.1837(3) 0.8848(2) 0.0375(7) Uani 1 1 d . . . . .
N7 N 0.1227(2) 0.3448(2) 0.6805(2) 0.0265(5) Uani 1 1 d . . . . .
N2 N 0.2958(2) 0.3646(2) 0.5382(2) 0.0233(5) Uani 1 1 d . . . . .
N3 N 0.4508(2) 0.2668(2) 0.68849(19) 0.0212(5) Uani 1 1 d . . . . .
N8 N -0.0284(3) 0.3483(3) 0.7707(3) 0.0447(7) Uani 1 1 d . . . . .
N5 N 0.2393(2) 0.2201(2) 0.7821(2) 0.0240(5) Uani 1 1 d . . . . .
N1 N 0.2116(2) 0.1449(2) 0.5353(2) 0.0229(5) Uani 1 1 d . . . . .
C6 C 0.1864(3) 0.2174(4) 0.2315(3) 0.0403(8) Uani 1 1 d . . . . .
H6 H 0.181001 0.235005 0.162719 0.048 Uiso 1 1 calc R U . . .
C28 C 0.0729(3) 0.3131(3) 0.7600(3) 0.0284(6) Uani 1 1 d . . . . .
C2 C 0.1238(3) -0.0600(3) 0.4374(3) 0.0335(7) Uani 1 1 d . . . . .
H2 H 0.098482 -0.137754 0.440501 0.040 Uiso 1 1 calc R U . . .
C17 C 0.7148(3) 0.4575(3) 0.8864(3) 0.0328(7) Uani 1 1 d . . . . .
H17 H 0.794810 0.455240 0.909249 0.039 Uiso 1 1 calc R U . . .
C22 C 0.3136(3) 0.5539(3) 0.8351(3) 0.0315(7) Uani 1 1 d . . . . .
H22 H 0.232644 0.552009 0.812248 0.038 Uiso 1 1 calc R U . . .
C16 C 0.6436(3) 0.3568(3) 0.8000(2) 0.0269(6) Uani 1 1 d . . . . .
C23 C 0.4768(3) 0.4619(3) 0.8235(2) 0.0233(6) Uani 1 1 d . . . . .
C9 C 0.3440(3) 0.5063(3) 0.4449(3) 0.0344(7) Uani 1 1 d . . . . .
H9 H 0.378825 0.584538 0.449962 0.041 Uiso 1 1 calc R U . . .
C20 C 0.4963(3) 0.6618(3) 0.9506(3) 0.0373(8) Uani 1 1 d . . . . .
H20 H 0.541547 0.731941 1.005391 0.045 Uiso 1 1 calc R U . . .
C11 C 0.2460(2) 0.2828(3) 0.4358(2) 0.0240(6) Uani 1 1 d . . . . .
C15 C 0.6870(3) 0.2546(3) 0.7405(3) 0.0319(7) Uani 1 1 d . . . . .
H15 H 0.767075 0.249110 0.757729 0.038 Uiso 1 1 calc R U . . .
C3 C 0.1113(3) -0.0388(3) 0.3359(3) 0.0330(7) Uani 1 1 d . . . . .
H3 H 0.077021 -0.102024 0.268470 0.040 Uiso 1 1 calc R U . . .
C5 C 0.1417(3) 0.1066(4) 0.2302(3) 0.0404(8) Uani 1 1 d . . . . .
H5 H 0.104867 0.047811 0.160664 0.049 Uiso 1 1 calc R U . . .
C30 C 0.0467(3) 0.4068(3) 0.6377(3) 0.0392(8) Uani 1 1 d . . . . .
H30 H 0.055972 0.442549 0.580953 0.047 Uiso 1 1 calc R U . . .
C29 C -0.0443(3) 0.4075(4) 0.6919(4) 0.0535(11) Uani 1 1 d . . . . .
H29 H -0.110399 0.443897 0.677593 0.064 Uiso 1 1 calc R U . . .
C8 C 0.2937(3) 0.4238(3) 0.3417(3) 0.0358(7) Uani 1 1 d . . . . .
H8 H 0.294187 0.445064 0.275151 0.043 Uiso 1 1 calc R U . . .
C1 C 0.1746(3) 0.0345(3) 0.5367(3) 0.0274(6) Uani 1 1 d . . . . .
H1 H 0.182693 0.019363 0.606729 0.033 Uiso 1 1 calc R U . . .
C19 C 0.5488(3) 0.5619(3) 0.9051(2) 0.0298(7) Uani 1 1 d . . . . .
C24 C 0.5254(2) 0.3592(3) 0.7700(2) 0.0220(6) Uani 1 1 d . . . . .
C21 C 0.3800(4) 0.6577(3) 0.9158(3) 0.0382(8) Uani 1 1 d . . . . .
H21 H 0.344080 0.725090 0.946171 0.046 Uiso 1 1 calc R U . . .
C25 C 0.2778(3) 0.1414(3) 0.8346(3) 0.0320(7) Uani 1 1 d . . . . .
H25 H 0.347110 0.107690 0.828479 0.038 Uiso 1 1 calc R U . . .
C14 C 0.6122(3) 0.1637(3) 0.6576(3) 0.0326(7) Uani 1 1 d . . . . .
H14 H 0.640625 0.095225 0.616123 0.039 Uiso 1 1 calc R U . . .
C18 C 0.6699(3) 0.5559(3) 0.9358(3) 0.0354(8) Uani 1 1 d . . . . .
H18 H 0.719259 0.622189 0.991929 0.043 Uiso 1 1 calc R U . . .
C27 C 0.1364(3) 0.2415(3) 0.8147(2) 0.0268(6) Uani 1 1 d . . . . .
C26 C 0.1978(4) 0.1207(3) 0.8971(3) 0.0406(8) Uani 1 1 d . . . . .
H26 H 0.203330 0.070006 0.942653 0.049 Uiso 1 1 calc R U . . .
C7 C 0.2415(3) 0.3084(3) 0.3344(3) 0.0311(7) Uani 1 1 d . . . . .
C12 C 0.2002(2) 0.1654(3) 0.4345(2) 0.0235(6) Uani 1 1 d . . . . .
C4 C 0.1491(3) 0.0765(3) 0.3320(3) 0.0298(6) Uani 1 1 d . . . . .
C10 C 0.3435(3) 0.4738(3) 0.5422(3) 0.0286(6) Uani 1 1 d . . . . .
H10 H 0.378186 0.531192 0.613194 0.034 Uiso 1 1 calc R U . . .
C13 C 0.4937(3) 0.1718(3) 0.6341(3) 0.0275(6) Uani 1 1 d . . . . .
H13 H 0.442582 0.107293 0.577473 0.033 Uiso 1 1 calc R U . . .
S1 S 0.52602(7) 0.14189(7) 0.32353(7) 0.0350(2) Uani 1 1 d . . . . .
F2 F 0.5700(2) 0.0768(2) 0.11926(19) 0.0485(5) Uani 1 1 d . . . . .
F1 F 0.3962(2) 0.1112(3) 0.1264(2) 0.0609(7) Uani 1 1 d . . . . .
F3 F 0.4454(2) -0.0512(2) 0.14877(18) 0.0495(6) Uani 1 1 d . . . . .
O2 O 0.6226(2) 0.0851(3) 0.3539(2) 0.0543(8) Uani 1 1 d . . . . .
O3 O 0.4252(2) 0.1151(3) 0.3683(2) 0.0429(6) Uani 1 1 d . . . . .
O1 O 0.5565(4) 0.2648(3) 0.3304(3) 0.0752(11) Uani 1 1 d . . . . .
C1T C 0.4811(3) 0.0664(3) 0.1720(3) 0.0353(7) Uani 1 1 d . . . . .
O2S O 0.8087(4) 0.3191(5) 0.3367(7) 0.118(2) Uani 1 1 d . . . . .
H2S H 0.752291 0.293131 0.361265 0.177 Uiso 1 1 calc R U . . .
C1S C 0.8884(5) 0.2458(6) 0.3328(6) 0.0804(16) Uani 1 1 d . . . . .
H1SA H 0.870709 0.182165 0.259682 0.121 Uiso 1 1 calc R U . . .
H1SB H 0.886637 0.209896 0.392970 0.121 Uiso 1 1 calc R U . . .
H1SC H 0.965882 0.291857 0.342784 0.121 Uiso 1 1 calc R U . . .
O4S O -0.0558(7) 0.1343(8) 1.0042(7) 0.076(2) Uiso 0.5 1 d . . P A 1
H4S H -0.039929 0.100805 0.940988 0.114 Uiso 0.5 1 calc R U P A 1
C3S C -0.0995(13) 0.2339(14) 1.0027(13) 0.097(4) Uiso 0.5 1 d . . P A 1
H3SA H -0.124772 0.230890 0.924585 0.146 Uiso 0.5 1 calc R U P A 1
H3SB H -0.039373 0.304520 1.041541 0.146 Uiso 0.5 1 calc R U P A 1
H3SC H -0.166102 0.239235 1.040942 0.146 Uiso 0.5 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'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 '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'
S S 0.3331 0.5567 '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 0 0 0.0551
1 0 0 0.0551
0 -1 1 0.0697
0 1 -1 0.0887
1 0 2 0.0747
-1 0 -2 0.0747
-1 1 1 0.1244
1 -1 -1 0.1244
-1 0 2 0.0924
1 0 -2 0.0924
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
N4 Cr1 N2 92.83(10) . . ?
N4 Cr1 N3 79.90(10) . . ?
N7 Cr1 N4 91.56(10) . . ?
N7 Cr1 N2 93.18(10) . . ?
N7 Cr1 N3 169.81(10) . . ?
N7 Cr1 N5 81.42(10) . . ?
N7 Cr1 N1 92.61(10) . . ?
N2 Cr1 N3 92.79(9) . . ?
N5 Cr1 N4 94.30(10) . . ?
N5 Cr1 N2 171.16(10) . . ?
N5 Cr1 N3 93.59(9) . . ?
N5 Cr1 N1 92.83(10) . . ?
N1 Cr1 N4 172.20(9) . . ?
N1 Cr1 N2 80.37(10) . . ?
N1 Cr1 N3 96.52(9) . . ?
C22 N4 Cr1 128.0(2) . . ?
C22 N4 C23 118.6(3) . . ?
C23 N4 Cr1 113.41(19) . . ?
C27 N6 C26 104.2(3) . . ?
C28 N7 Cr1 114.1(2) . . ?
C28 N7 C30 105.0(3) . . ?
C30 N7 Cr1 140.7(2) . . ?
C11 N2 Cr1 112.38(19) . . ?
C10 N2 Cr1 128.9(2) . . ?
C10 N2 C11 118.7(3) . . ?
C24 N3 Cr1 112.70(19) . . ?
C13 N3 Cr1 128.9(2) . . ?
C13 N3 C24 118.4(2) . . ?
C28 N8 C29 102.7(3) . . ?
C25 N5 Cr1 140.7(2) . . ?
C27 N5 Cr1 113.9(2) . . ?
C27 N5 C25 105.2(3) . . ?
C1 N1 Cr1 128.6(2) . . ?
C1 N1 C12 118.6(3) . . ?
C12 N1 Cr1 112.71(19) . . ?
C5 C6 H6 119.4 . . ?
C5 C6 C7 121.1(3) . . ?
C7 C6 H6 119.4 . . ?
N7 C28 C27 115.1(3) . . ?
N8 C28 N7 114.3(3) . . ?
N8 C28 C27 130.5(3) . . ?
C3 C2 H2 120.3 . . ?
C3 C2 C1 119.5(3) . . ?
C1 C2 H2 120.3 . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C18 C17 C16 121.1(3) . . ?
N4 C22 H22 119.0 . . ?
N4 C22 C21 121.9(3) . . ?
C21 C22 H22 119.0 . . ?
C15 C16 C17 123.6(3) . . ?
C24 C16 C17 119.0(3) . . ?
C24 C16 C15 117.4(3) . . ?
N4 C23 C19 122.9(3) . . ?
N4 C23 C24 117.1(2) . . ?
C19 C23 C24 120.0(3) . . ?
C8 C9 H9 120.3 . . ?
C8 C9 C10 119.5(3) . . ?
C10 C9 H9 120.3 . . ?
C19 C20 H20 120.1 . . ?
C21 C20 H20 120.1 . . ?
C21 C20 C19 119.7(3) . . ?
N2 C11 C7 123.1(3) . . ?
N2 C11 C12 117.0(3) . . ?
C7 C11 C12 119.9(3) . . ?
C16 C15 H15 120.4 . . ?
C14 C15 C16 119.3(3) . . ?
C14 C15 H15 120.4 . . ?
C2 C3 H3 120.1 . . ?
C2 C3 C4 119.9(3) . . ?
C4 C3 H3 120.1 . . ?
C6 C5 H5 119.5 . . ?
C6 C5 C4 121.0(3) . . ?
C4 C5 H5 119.5 . . ?
N7 C30 H30 126.6 . . ?
C29 C30 N7 106.7(3) . . ?
C29 C30 H30 126.6 . . ?
N8 C29 H29 124.4 . . ?
C30 C29 N8 111.2(3) . . ?
C30 C29 H29 124.4 . . ?
C9 C8 H8 119.9 . . ?
C9 C8 C7 120.2(3) . . ?
C7 C8 H8 119.9 . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 H1 119.1 . . ?
C23 C19 C18 118.5(3) . . ?
C20 C19 C23 117.0(3) . . ?
C20 C19 C18 124.5(3) . . ?
N3 C24 C16 123.0(3) . . ?
N3 C24 C23 116.7(3) . . ?
C16 C24 C23 120.2(3) . . ?
C22 C21 H21 120.0 . . ?
C20 C21 C22 119.9(3) . . ?
C20 C21 H21 120.0 . . ?
N5 C25 H25 126.4 . . ?
C26 C25 N5 107.1(3) . . ?
C26 C25 H25 126.4 . . ?
C15 C14 H14 120.0 . . ?
C15 C14 C13 119.9(3) . . ?
C13 C14 H14 120.0 . . ?
C17 C18 C19 121.2(3) . . ?
C17 C18 H18 119.4 . . ?
C19 C18 H18 119.4 . . ?
N6 C27 N5 113.1(3) . . ?
N6 C27 C28 131.5(3) . . ?
N5 C27 C28 115.1(3) . . ?
N6 C26 H26 124.8 . . ?
C25 C26 N6 110.3(3) . . ?
C25 C26 H26 124.8 . . ?
C11 C7 C6 119.1(3) . . ?
C11 C7 C8 116.7(3) . . ?
C8 C7 C6 124.2(3) . . ?
N1 C12 C11 117.0(3) . . ?
N1 C12 C4 123.0(3) . . ?
C4 C12 C11 120.0(3) . . ?
C3 C4 C5 123.9(3) . . ?
C12 C4 C3 117.2(3) . . ?
C12 C4 C5 118.9(3) . . ?
N2 C10 C9 121.9(3) . . ?
N2 C10 H10 119.1 . . ?
C9 C10 H10 119.1 . . ?
N3 C13 C14 122.0(3) . . ?
N3 C13 H13 119.0 . . ?
C14 C13 H13 119.0 . . ?
O2 S1 C1T 103.07(16) . . ?
O3 S1 O2 114.05(18) . . ?
O3 S1 C1T 104.17(16) . . ?
O1 S1 O2 115.1(2) . . ?
O1 S1 O3 115.6(2) . . ?
O1 S1 C1T 102.53(19) . . ?
F2 C1T S1 110.9(2) . . ?
F2 C1T F3 106.5(3) . . ?
F1 C1T S1 112.4(3) . . ?
F1 C1T F2 107.3(3) . . ?
F1 C1T F3 108.1(3) . . ?
F3 C1T S1 111.3(2) . . ?
C1S O2S H2S 109.5 . . ?
O2S C1S H1SA 109.5 . . ?
O2S C1S H1SB 109.5 . . ?
O2S C1S H1SC 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C3S O4S H4S 109.5 . . ?
O4S C3S H3SA 109.5 . . ?
O4S C3S H3SB 109.5 . . ?
O4S C3S H3SC 109.5 . . ?
H3SA C3S H3SB 109.5 . . ?
H3SA C3S H3SC 109.5 . . ?
H3SB C3S H3SC 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 N4 2.067(3) . ?
Cr1 N7 1.993(3) . ?
Cr1 N2 2.069(2) . ?
Cr1 N3 2.086(2) . ?
Cr1 N5 2.000(2) . ?
Cr1 N1 2.063(2) . ?
N4 C22 1.327(4) . ?
N4 C23 1.364(4) . ?
N6 C27 1.329(4) . ?
N6 C26 1.374(5) . ?
N7 C28 1.361(4) . ?
N7 C30 1.369(4) . ?
N2 C11 1.365(4) . ?
N2 C10 1.334(4) . ?
N3 C24 1.370(4) . ?
N3 C13 1.327(4) . ?
N8 C28 1.319(4) . ?
N8 C29 1.385(6) . ?
N5 C25 1.375(4) . ?
N5 C27 1.363(4) . ?
N1 C1 1.337(4) . ?
N1 C12 1.361(4) . ?
C6 H6 0.9500 . ?
C6 C5 1.352(6) . ?
C6 C7 1.428(5) . ?
C28 C27 1.448(5) . ?
C2 H2 0.9500 . ?
C2 C3 1.372(5) . ?
C2 C1 1.407(4) . ?
C17 H17 0.9500 . ?
C17 C16 1.432(4) . ?
C17 C18 1.351(5) . ?
C22 H22 0.9500 . ?
C22 C21 1.401(5) . ?
C16 C15 1.413(5) . ?
C16 C24 1.393(4) . ?
C23 C19 1.406(4) . ?
C23 C24 1.429(4) . ?
C9 H9 0.9500 . ?
C9 C8 1.377(5) . ?
C9 C10 1.398(4) . ?
C20 H20 0.9500 . ?
C20 C19 1.404(5) . ?
C20 C21 1.367(6) . ?
C11 C7 1.402(4) . ?
C11 C12 1.429(4) . ?
C15 H15 0.9500 . ?
C15 C14 1.370(5) . ?
C3 H3 0.9500 . ?
C3 C4 1.406(5) . ?
C5 H5 0.9500 . ?
C5 C4 1.432(5) . ?
C30 H30 0.9500 . ?
C30 C29 1.356(6) . ?
C29 H29 0.9500 . ?
C8 H8 0.9500 . ?
C8 C7 1.404(5) . ?
C1 H1 0.9500 . ?
C19 C18 1.436(5) . ?
C21 H21 0.9500 . ?
C25 H25 0.9500 . ?
C25 C26 1.364(5) . ?
C14 H14 0.9500 . ?
C14 C13 1.403(4) . ?
C18 H18 0.9500 . ?
C26 H26 0.9500 . ?
C12 C4 1.403(4) . ?
C10 H10 0.9500 . ?
C13 H13 0.9500 . ?
S1 O2 1.444(3) . ?
S1 O3 1.434(3) . ?
S1 O1 1.432(3) . ?
S1 C1T 1.827(4) . ?
F2 C1T 1.337(4) . ?
F1 C1T 1.320(4) . ?
F3 C1T 1.338(4) . ?
O2S H2S 0.8400 . ?
O2S C1S 1.343(7) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
O4S H4S 0.8400 . ?
O4S C3S 1.342(16) . ?
C3S H3SA 0.9800 . ?
C3S H3SB 0.9800 . ?
C3S H3SC 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
O2S H2S O1 0.84 2.25 2.951(6) 141.1 . 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 N4 C22 C21 -179.4(2) . . . . ?
Cr1 N4 C23 C19 -179.6(2) . . . . ?
Cr1 N4 C23 C24 1.9(3) . . . . ?
Cr1 N7 C28 N8 177.3(2) . . . . ?
Cr1 N7 C28 C27 -5.7(3) . . . . ?
Cr1 N7 C30 C29 -176.0(3) . . . . ?
Cr1 N2 C11 C7 177.1(2) . . . . ?
Cr1 N2 C11 C12 -4.8(3) . . . . ?
Cr1 N2 C10 C9 -177.5(2) . . . . ?
Cr1 N3 C24 C16 178.0(2) . . . . ?
Cr1 N3 C24 C23 -3.1(3) . . . . ?
Cr1 N3 C13 C14 -179.3(2) . . . . ?
Cr1 N5 C25 C26 -174.6(2) . . . . ?
Cr1 N5 C27 N6 176.6(2) . . . . ?
Cr1 N5 C27 C28 1.8(3) . . . . ?
Cr1 N1 C1 C2 176.1(2) . . . . ?
Cr1 N1 C12 C11 6.0(3) . . . . ?
Cr1 N1 C12 C4 -175.7(2) . . . . ?
N4 C22 C21 C20 -0.6(5) . . . . ?
N4 C23 C19 C20 -1.2(4) . . . . ?
N4 C23 C19 C18 179.1(3) . . . . ?
N4 C23 C24 N3 0.8(4) . . . . ?
N4 C23 C24 C16 179.8(2) . . . . ?
N7 C28 C27 N6 -171.0(3) . . . . ?
N7 C28 C27 N5 2.5(4) . . . . ?
N7 C30 C29 N8 0.8(5) . . . . ?
N2 C11 C7 C6 -179.3(3) . . . . ?
N2 C11 C7 C8 1.3(4) . . . . ?
N2 C11 C12 N1 -0.8(4) . . . . ?
N2 C11 C12 C4 -179.2(3) . . . . ?
N8 C28 C27 N6 5.4(6) . . . . ?
N8 C28 C27 N5 179.0(3) . . . . ?
N5 C25 C26 N6 0.6(4) . . . . ?
N1 C12 C4 C3 -1.5(4) . . . . ?
N1 C12 C4 C5 -179.6(3) . . . . ?
C6 C5 C4 C3 -175.8(3) . . . . ?
C6 C5 C4 C12 2.2(5) . . . . ?
C28 N7 C30 C29 -0.9(4) . . . . ?
C28 N8 C29 C30 -0.4(5) . . . . ?
C2 C3 C4 C5 178.8(3) . . . . ?
C2 C3 C4 C12 0.7(5) . . . . ?
C17 C16 C15 C14 -178.7(3) . . . . ?
C17 C16 C24 N3 -179.9(2) . . . . ?
C17 C16 C24 C23 1.2(4) . . . . ?
C22 N4 C23 C19 0.8(4) . . . . ?
C22 N4 C23 C24 -177.7(2) . . . . ?
C16 C17 C18 C19 1.2(5) . . . . ?
C16 C15 C14 C13 -1.1(5) . . . . ?
C23 N4 C22 C21 0.2(4) . . . . ?
C23 C19 C18 C17 1.2(4) . . . . ?
C9 C8 C7 C6 179.5(3) . . . . ?
C9 C8 C7 C11 -1.2(5) . . . . ?
C20 C19 C18 C17 -178.4(3) . . . . ?
C11 N2 C10 C9 -0.2(4) . . . . ?
C11 C12 C4 C3 176.7(3) . . . . ?
C11 C12 C4 C5 -1.4(4) . . . . ?
C15 C16 C24 N3 1.5(4) . . . . ?
C15 C16 C24 C23 -177.4(2) . . . . ?
C15 C14 C13 N3 1.3(5) . . . . ?
C3 C2 C1 N1 -0.3(5) . . . . ?
C5 C6 C7 C11 -1.9(5) . . . . ?
C5 C6 C7 C8 177.5(3) . . . . ?
C30 N7 C28 N8 0.7(4) . . . . ?
C30 N7 C28 C27 177.7(3) . . . . ?
C29 N8 C28 N7 -0.2(4) . . . . ?
C29 N8 C28 C27 -176.6(4) . . . . ?
C8 C9 C10 N2 0.2(5) . . . . ?
C1 N1 C12 C11 -177.0(3) . . . . ?
C1 N1 C12 C4 1.3(4) . . . . ?
C1 C2 C3 C4 0.1(5) . . . . ?
C19 C23 C24 N3 -177.7(2) . . . . ?
C19 C23 C24 C16 1.2(4) . . . . ?
C19 C20 C21 C22 0.1(5) . . . . ?
C24 N3 C13 C14 -0.1(4) . . . . ?
C24 C16 C15 C14 -0.2(4) . . . . ?
C24 C23 C19 C20 177.2(3) . . . . ?
C24 C23 C19 C18 -2.4(4) . . . . ?
C21 C20 C19 C23 0.7(4) . . . . ?
C21 C20 C19 C18 -179.6(3) . . . . ?
C25 N5 C27 N6 0.9(3) . . . . ?
C25 N5 C27 C28 -173.8(3) . . . . ?
C18 C17 C16 C15 176.0(3) . . . . ?
C18 C17 C16 C24 -2.4(4) . . . . ?
C27 N6 C26 C25 -0.1(4) . . . . ?
C27 N5 C25 C26 -0.9(3) . . . . ?
C26 N6 C27 N5 -0.6(3) . . . . ?
C26 N6 C27 C28 173.1(3) . . . . ?
C7 C6 C5 C4 -0.5(6) . . . . ?
C7 C11 C12 N1 177.3(3) . . . . ?
C7 C11 C12 C4 -1.0(4) . . . . ?
C12 N1 C1 C2 -0.4(4) . . . . ?
C12 C11 C7 C6 2.6(4) . . . . ?
C12 C11 C7 C8 -176.8(3) . . . . ?
C10 N2 C11 C7 -0.6(4) . . . . ?
C10 N2 C11 C12 177.5(3) . . . . ?
C10 C9 C8 C7 0.5(5) . . . . ?
C13 N3 C24 C16 -1.4(4) . . . . ?
C13 N3 C24 C23 177.6(2) . . . . ?
O2 S1 C1T F2 -56.4(3) . . . . ?
O2 S1 C1T F1 -176.5(3) . . . . ?
O2 S1 C1T F3 62.1(3) . . . . ?
O3 S1 C1T F2 -175.7(2) . . . . ?
O3 S1 C1T F1 64.2(3) . . . . ?
O3 S1 C1T F3 -57.3(3) . . . . ?
O1 S1 C1T F2 63.5(3) . . . . ?
O1 S1 C1T F1 -56.7(3) . . . . ?
O1 S1 C1T F3 -178.1(3) . . . . ?
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
-1.0000 0.0004 -0.0005 0.0642 0.0872 0.0791
1.0000 -0.0004 0.0005 -0.0642 -0.0872 -0.0791
-0.0001 -0.9993 1.0012 0.1066 -0.1101 0.0311
0.0001 0.9993 -1.0012 -0.1066 0.1101 -0.0311
1.0011 0.0013 1.9994 0.1244 -0.1525 -0.2448
-1.0011 -0.0013 -1.9994 -0.1244 0.1525 0.2448
-0.9987 1.0015 0.9972 0.1461 0.1321 -0.1176
0.9987 -1.0015 -0.9972 -0.1461 -0.1321 0.1176
-0.9988 0.0022 1.9984 0.2528 0.0220 -0.0865
0.9988 -0.0022 -1.9984 -0.2528 -0.0220 0.0865
