#------------------------------------------------------------------------------
#$Date: 2022-03-12 00:54:49 +0200 (Sat, 12 Mar 2022) $
#$Revision: 273666 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/98/7129820.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_7129820
loop_
_publ_author_name
'Kooij, Bastiaan'
'Dong, Zhaowen'
'Varava, Paul'
'Fadaei-Tirani, Farzaneh'
'Scopelliti, Rosario'
'Piveteau, Laura'
'Severin, Kay'
_publ_section_title
;
 Vanadium complexes with N-heterocyclic vinylidene ligands
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC00768A
_journal_year                    2022
_chemical_formula_moiety         'C28 H36 Cl3 N2 V, C6 H6'
_chemical_formula_sum            'C34 H42 Cl3 N2 V'
_chemical_formula_weight         635.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-08-27 deposited with the CCDC.	2022-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.312(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7785(3)
_cell_length_b                   9.29150(18)
_cell_length_c                   22.4036(4)
_cell_measurement_reflns_used    7502
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      72.5500
_cell_measurement_theta_min      3.6830
_cell_volume                     3398.82(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.113a (Rigaku OD, 2021)'
_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, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -16.00  30.00   1.00   12.50    --  -43.50  81.00-130.00   46
  2  ω      3.00  28.00   1.00   12.50    --   43.68 -81.00 106.00   25
  3  ω     52.00 101.00   1.00   50.00    --  103.26 -81.00 106.00   49
  4  ω    106.00 178.00   1.00   50.00    --  103.26  81.00-130.00   72
  5  ω    -59.00  -6.00   1.00   12.50    --  -43.50 125.00 -60.00   53
  6  ω   -103.00 -18.00   1.00   12.50    --  -43.50 -57.00  60.00   85
  7  ω      7.00  84.00   1.00   12.50    --   43.68 -99.00 -90.00   77
  8  ω    103.00 175.00   1.00   50.00    --  103.26  77.00  90.00   72
  9  ω    116.00 148.00   1.00   50.00    --  103.26 125.00 -90.00   32
 10  ω     34.00  84.00   1.00   50.00    --  103.26 -61.00 -30.00   50
 11  ω    115.00 176.00   1.00   50.00    --  103.26  77.00 -60.00   61
 12  ω    116.00 143.00   1.00   50.00    --  103.26 125.00  30.00   27
 13  ω     86.00 166.00   1.00   50.00    --  103.26  45.00-150.00   80
 14  ω    134.00 159.00   1.00   50.00    --  103.26  77.00 120.00   25
 15  ω     40.00  67.00   1.00   50.00    --  103.26-125.00  90.00   27
 16  ω     99.00 125.00   1.00   50.00    --  103.26 -77.00 -90.00   26
;
_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      -0.0356587000
_diffrn_orient_matrix_UB_12      -0.0837573000
_diffrn_orient_matrix_UB_13      -0.0594811000
_diffrn_orient_matrix_UB_21      -0.0862235000
_diffrn_orient_matrix_UB_22      0.0112881000
_diffrn_orient_matrix_UB_23      0.0126685000
_diffrn_orient_matrix_UB_31      -0.0140823000
_diffrn_orient_matrix_UB_32      0.1425767000
_diffrn_orient_matrix_UB_33      -0.0360194000
_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     0.0336
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17167
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.529
_diffrn_reflns_theta_min         3.737
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.784
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.712
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.113a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on Gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics
as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_density_diffrn    1.243
_exptl_crystal_description       plate
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.055
_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     400
_refine_ls_number_reflns         6581
_refine_ls_number_restraints     174
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0484P)²+1.9668P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1017
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5506
_reflns_number_total             6581
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2cc00768a2.cif
_cod_data_source_block           bk122
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Gaussian' was
changed to 'gaussian' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3398.82(12)
_cod_database_code               7129820
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C34 H42 Cl3 N2 V'
_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   0.910
_shelx_estimated_absorpt_t_min   0.621
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Uiso/Uaniso restraints and constraints
C31A \\sim C31B \\sim C32A \\sim C32B \\sim C33A \\sim C33B \\sim C34A \\sim
C34B \\sim C35A \\sim C35B \\sim C36A \\sim C36B: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
3. Others
 Sof(C31B)=Sof(H31B)=Sof(C32B)=Sof(H32B)=Sof(C33B)=Sof(H33B)=Sof(C34B)=
 Sof(H34B)=Sof(C35B)=Sof(H35B)=Sof(C36B)=Sof(H36B)=1-FVAR(1)
 Sof(C31A)=Sof(H31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=
 Sof(H34A)=Sof(C35A)=Sof(H35A)=Sof(C36A)=Sof(H36A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C25(H25), C28(H28)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C21(H21), C22(H22), C23(H23),
 C31A(H31A), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A),
 C31B(H31B), C32B(H32B), C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B)
4.c Fitted hexagon refined as free rotating group:
 C31A(C32A,C33A,C34A,C35A,C36A), C31B(C32B,C33B,C34B,C35B,C36B)
4.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C)
;
_olex2_date_sample_data_collection 2021-08-26
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.156
_oxdiff_exptl_absorpt_empirical_full_min 0.891
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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
V1 V 0.28092(2) 0.43353(4) 0.58258(2) 0.01938(10) Uani 1 1 d . . . . .
Cl1 Cl 0.40611(3) 0.37415(6) 0.63150(3) 0.03454(14) Uani 1 1 d . . . . .
Cl2 Cl 0.25178(3) 0.34303(6) 0.48888(2) 0.02816(13) Uani 1 1 d . . . . .
Cl3 Cl 0.18572(3) 0.36975(6) 0.63092(3) 0.03010(13) Uani 1 1 d . . . . .
N1 N 0.20902(10) 0.85148(19) 0.56531(8) 0.0216(4) Uani 1 1 d . . . . .
N2 N 0.34052(11) 0.85878(19) 0.57310(8) 0.0222(4) Uani 1 1 d . . . . .
C2 C 0.27667(12) 0.7680(2) 0.57167(9) 0.0202(4) Uani 1 1 d . . . . .
C4 C 0.31239(14) 0.9983(2) 0.56685(11) 0.0286(5) Uani 1 1 d . . . . .
H4 H 0.344501 1.082227 0.566055 0.034 Uiso 1 1 calc R U . . .
C5 C 0.23044(14) 0.9940(2) 0.56206(11) 0.0279(5) Uani 1 1 d . . . . .
H5 H 0.194447 1.074259 0.557329 0.033 Uiso 1 1 calc R U . . .
C6 C 0.27923(12) 0.6165(2) 0.57601(10) 0.0220(4) Uani 1 1 d . . . . .
C7 C 0.12810(12) 0.7947(2) 0.56278(10) 0.0236(4) Uani 1 1 d . . . . .
C8 C 0.10823(13) 0.7582(2) 0.61813(11) 0.0255(5) Uani 1 1 d . . . . .
C9 C 0.03082(14) 0.6988(3) 0.61365(12) 0.0340(5) Uani 1 1 d . . . . .
H9 H 0.014446 0.671939 0.649965 0.041 Uiso 1 1 calc R U . . .
C10 C -0.02257(15) 0.6782(3) 0.55732(14) 0.0412(6) Uani 1 1 d . . . . .
H10 H -0.074822 0.636699 0.555451 0.049 Uiso 1 1 calc R U . . .
C11 C -0.00110(15) 0.7169(3) 0.50431(13) 0.0384(6) Uani 1 1 d . . . . .
H11 H -0.038948 0.702258 0.466151 0.046 Uiso 1 1 calc R U . . .
C12 C 0.07527(14) 0.7775(3) 0.50499(11) 0.0300(5) Uani 1 1 d . . . . .
C13 C 0.16643(14) 0.7865(3) 0.67986(11) 0.0296(5) Uani 1 1 d . . . . .
H13 H 0.223693 0.775808 0.674520 0.036 Uiso 1 1 calc R U . . .
C14 C 0.15606(19) 0.9406(3) 0.70021(13) 0.0429(6) Uani 1 1 d . . . . .
H14A H 0.099805 0.954600 0.704609 0.064 Uiso 1 1 calc R U . . .
H14B H 0.167366 1.007730 0.669434 0.064 Uiso 1 1 calc R U . . .
H14C H 0.194355 0.958586 0.739664 0.064 Uiso 1 1 calc R U . . .
C15 C 0.15549(17) 0.6824(3) 0.73019(12) 0.0382(6) Uani 1 1 d . . . . .
H15A H 0.200125 0.696046 0.766579 0.057 Uiso 1 1 calc R U . . .
H15B H 0.156398 0.583201 0.715488 0.057 Uiso 1 1 calc R U . . .
H15C H 0.102945 0.701193 0.740771 0.057 Uiso 1 1 calc R U . . .
C16 C 0.09925(17) 0.8177(3) 0.44599(11) 0.0368(6) Uani 1 1 d . . . . .
H16 H 0.148853 0.880619 0.456725 0.044 Uiso 1 1 calc R U . . .
C17 C 0.0316(2) 0.9024(4) 0.40333(15) 0.0575(8) Uani 1 1 d . . . . .
H17A H -0.016838 0.841015 0.390287 0.086 Uiso 1 1 calc R U . . .
H17B H 0.050639 0.933852 0.367257 0.086 Uiso 1 1 calc R U . . .
H17C H 0.017322 0.986714 0.425012 0.086 Uiso 1 1 calc R U . . .
C18 C 0.1212(3) 0.6853(4) 0.41329(16) 0.0727(12) Uani 1 1 d . . . . .
H18A H 0.165880 0.633205 0.440693 0.109 Uiso 1 1 calc R U . . .
H18B H 0.138781 0.714955 0.376330 0.109 Uiso 1 1 calc R U . . .
H18C H 0.073262 0.622447 0.401780 0.109 Uiso 1 1 calc R U . . .
C19 C 0.42435(13) 0.8125(2) 0.57912(11) 0.0230(4) Uani 1 1 d . . . . .
C20 C 0.47582(14) 0.8093(2) 0.63773(11) 0.0258(5) Uani 1 1 d . . . . .
C21 C 0.55500(15) 0.7596(3) 0.64197(12) 0.0324(5) Uani 1 1 d . . . . .
H21 H 0.592085 0.755141 0.680984 0.039 Uiso 1 1 calc R U . . .
C22 C 0.58086(15) 0.7165(3) 0.59040(12) 0.0339(5) Uani 1 1 d . . . . .
H22 H 0.634993 0.681158 0.594538 0.041 Uiso 1 1 calc R U . . .
C23 C 0.52888(15) 0.7242(3) 0.53316(12) 0.0322(5) Uani 1 1 d . . . . .
H23 H 0.547686 0.694388 0.498231 0.039 Uiso 1 1 calc R U . . .
C24 C 0.44927(14) 0.7750(2) 0.52575(11) 0.0254(5) Uani 1 1 d . . . . .
C25 C 0.44776(15) 0.8541(3) 0.69479(11) 0.0309(5) Uani 1 1 d . . . . .
H25 H 0.397308 0.913998 0.681210 0.037 Uiso 1 1 calc R U . . .
C26 C 0.4250(2) 0.7243(3) 0.72812(14) 0.0507(8) Uani 1 1 d . . . . .
H26A H 0.402862 0.756333 0.762744 0.076 Uiso 1 1 calc R U . . .
H26B H 0.473769 0.665113 0.743336 0.076 Uiso 1 1 calc R U . . .
H26C H 0.383554 0.667433 0.699874 0.076 Uiso 1 1 calc R U . . .
C27 C 0.5115(2) 0.9463(4) 0.73723(16) 0.0577(9) Uani 1 1 d . . . . .
H27A H 0.561750 0.890219 0.751509 0.087 Uiso 1 1 calc R U . . .
H27B H 0.490343 0.976550 0.772547 0.087 Uiso 1 1 calc R U . . .
H27C H 0.523449 1.031400 0.714987 0.087 Uiso 1 1 calc R U . . .
C28 C 0.39334(15) 0.7882(3) 0.46207(11) 0.0309(5) Uani 1 1 d . . . . .
H28 H 0.341859 0.837963 0.465798 0.037 Uiso 1 1 calc R U . . .
C29 C 0.43437(18) 0.8781(3) 0.42056(13) 0.0428(6) Uani 1 1 d . . . . .
H29A H 0.450039 0.971888 0.439689 0.064 Uiso 1 1 calc R U . . .
H29B H 0.396068 0.892100 0.380780 0.064 Uiso 1 1 calc R U . . .
H29C H 0.483330 0.827994 0.414567 0.064 Uiso 1 1 calc R U . . .
C30 C 0.3710(2) 0.6404(3) 0.43370(14) 0.0538(8) Uani 1 1 d . . . . .
H30A H 0.420517 0.592278 0.427733 0.081 Uiso 1 1 calc R U . . .
H30B H 0.332014 0.651433 0.394024 0.081 Uiso 1 1 calc R U . . .
H30C H 0.345995 0.582532 0.461104 0.081 Uiso 1 1 calc R U . . .
C31A C 0.60478(18) 0.3429(4) 0.77810(16) 0.0724(11) Uani 0.785(5) 1 d G U P A 1
H31A H 0.554944 0.290940 0.773439 0.087 Uiso 0.785(5) 1 calc R U P A 1
C32A C 0.6614(2) 0.3429(5) 0.83421(14) 0.0770(11) Uani 0.785(5) 1 d G U P A 1
H32A H 0.650186 0.291009 0.867909 0.092 Uiso 0.785(5) 1 calc R U P A 1
C33A C 0.73427(19) 0.4189(5) 0.84103(12) 0.0807(12) Uani 0.785(5) 1 d G U P A 1
H33A H 0.772934 0.418880 0.879385 0.097 Uiso 0.785(5) 1 calc R U P A 1
C34A C 0.75061(16) 0.4948(4) 0.79173(16) 0.0825(13) Uani 0.785(5) 1 d G U P A 1
H34A H 0.800441 0.546684 0.796391 0.099 Uiso 0.785(5) 1 calc R U P A 1
C35A C 0.69403(18) 0.4947(5) 0.73561(13) 0.0702(12) Uani 0.785(5) 1 d G U P A 1
H35A H 0.705201 0.546617 0.701920 0.084 Uiso 0.785(5) 1 calc R U P A 1
C36A C 0.62112(17) 0.4188(5) 0.72880(11) 0.0702(11) Uani 0.785(5) 1 d G U P A 1
H36A H 0.582452 0.418746 0.690443 0.084 Uiso 0.785(5) 1 calc R U P A 1
C31B C 0.6180(8) 0.3356(15) 0.7527(6) 0.0761(16) Uani 0.215(5) 1 d G U P A 2
H31B H 0.581869 0.273506 0.725448 0.091 Uiso 0.215(5) 1 calc R U P A 2
C32B C 0.6517(9) 0.2919(13) 0.8125(6) 0.0770(16) Uani 0.215(5) 1 d G U P A 2
H32B H 0.638618 0.199928 0.826160 0.092 Uiso 0.215(5) 1 calc R U P A 2
C33B C 0.7046(9) 0.3827(16) 0.8524(4) 0.0778(18) Uani 0.215(5) 1 d G U P A 2
H33B H 0.727632 0.352828 0.893274 0.093 Uiso 0.215(5) 1 calc R U P A 2
C34B C 0.7238(8) 0.5172(15) 0.8324(6) 0.0793(16) Uani 0.215(5) 1 d G U P A 2
H34B H 0.759897 0.579309 0.859676 0.095 Uiso 0.215(5) 1 calc R U P A 2
C35B C 0.6901(8) 0.5609(13) 0.7726(6) 0.0773(16) Uani 0.215(5) 1 d G U P A 2
H35B H 0.703150 0.652890 0.758965 0.093 Uiso 0.215(5) 1 calc R U P A 2
C36B C 0.6372(9) 0.4701(16) 0.7327(4) 0.0749(16) Uani 0.215(5) 1 d G U P A 2
H36B H 0.614136 0.499991 0.691850 0.090 Uiso 0.215(5) 1 calc R U P A 2
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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 '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 -1 0.0270
-1 0 1 0.0489
0 1 0 0.0130
0 -1 0 0.0059
-1 0 0 0.0366
1 -2 2 0.0251
2 0 -1 0.0279
1 0 2 0.0543
-1 0 -2 0.0315
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 V1 Cl2 110.75(3) . . ?
Cl1 V1 Cl3 113.78(3) . . ?
Cl3 V1 Cl2 109.71(3) . . ?
C6 V1 Cl1 106.70(7) . . ?
C6 V1 Cl2 107.55(8) . . ?
C6 V1 Cl3 108.08(7) . . ?
C2 N1 C5 109.45(18) . . ?
C2 N1 C7 123.51(18) . . ?
C5 N1 C7 127.04(18) . . ?
C2 N2 C4 109.42(18) . . ?
C2 N2 C19 124.21(18) . . ?
C4 N2 C19 126.36(18) . . ?
N1 C2 N2 106.53(18) . . ?
N1 C2 C6 126.13(19) . . ?
N2 C2 C6 127.34(19) . . ?
N2 C4 H4 126.3 . . ?
C5 C4 N2 107.35(19) . . ?
C5 C4 H4 126.3 . . ?
N1 C5 H5 126.4 . . ?
C4 C5 N1 107.25(19) . . ?
C4 C5 H5 126.4 . . ?
C2 C6 V1 178.59(19) . . ?
C8 C7 N1 117.87(19) . . ?
C8 C7 C12 124.3(2) . . ?
C12 C7 N1 117.8(2) . . ?
C7 C8 C13 122.0(2) . . ?
C9 C8 C7 116.2(2) . . ?
C9 C8 C13 121.8(2) . . ?
C8 C9 H9 119.4 . . ?
C10 C9 C8 121.2(2) . . ?
C10 C9 H9 119.4 . . ?
C9 C10 H10 119.6 . . ?
C11 C10 C9 120.8(2) . . ?
C11 C10 H10 119.6 . . ?
C10 C11 H11 119.3 . . ?
C10 C11 C12 121.4(2) . . ?
C12 C11 H11 119.3 . . ?
C7 C12 C16 122.7(2) . . ?
C11 C12 C7 116.1(2) . . ?
C11 C12 C16 121.2(2) . . ?
C8 C13 H13 107.9 . . ?
C8 C13 C14 109.9(2) . . ?
C8 C13 C15 113.6(2) . . ?
C14 C13 H13 107.9 . . ?
C14 C13 C15 109.4(2) . . ?
C15 C13 H13 107.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 C16 H16 107.9 . . ?
C12 C16 C17 111.4(2) . . ?
C12 C16 C18 111.3(2) . . ?
C17 C16 H16 107.9 . . ?
C18 C16 H16 107.9 . . ?
C18 C16 C17 110.1(3) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C20 C19 N2 118.13(19) . . ?
C20 C19 C24 123.8(2) . . ?
C24 C19 N2 118.0(2) . . ?
C19 C20 C25 122.8(2) . . ?
C21 C20 C19 116.5(2) . . ?
C21 C20 C25 120.7(2) . . ?
C20 C21 H21 119.4 . . ?
C22 C21 C20 121.2(2) . . ?
C22 C21 H21 119.4 . . ?
C21 C22 H22 119.7 . . ?
C23 C22 C21 120.6(2) . . ?
C23 C22 H22 119.7 . . ?
C22 C23 H23 119.5 . . ?
C22 C23 C24 120.9(2) . . ?
C24 C23 H23 119.5 . . ?
C19 C24 C28 122.7(2) . . ?
C23 C24 C19 116.8(2) . . ?
C23 C24 C28 120.5(2) . . ?
C20 C25 H25 107.5 . . ?
C20 C25 C27 111.8(2) . . ?
C26 C25 C20 111.1(2) . . ?
C26 C25 H25 107.5 . . ?
C26 C25 C27 111.2(3) . . ?
C27 C25 H25 107.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C24 C28 H28 108.5 . . ?
C24 C28 C29 110.4(2) . . ?
C24 C28 C30 111.0(2) . . ?
C29 C28 H28 108.5 . . ?
C30 C28 H28 108.5 . . ?
C30 C28 C29 110.0(2) . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32A C31A H31A 120.0 . . ?
C32A C31A C36A 120.0 . . ?
C36A C31A H31A 120.0 . . ?
C31A C32A H32A 120.0 . . ?
C33A C32A C31A 120.0 . . ?
C33A C32A H32A 120.0 . . ?
C32A C33A H33A 120.0 . . ?
C32A C33A C34A 120.0 . . ?
C34A C33A H33A 120.0 . . ?
C33A C34A H34A 120.0 . . ?
C33A C34A C35A 120.0 . . ?
C35A C34A H34A 120.0 . . ?
C34A C35A H35A 120.0 . . ?
C36A C35A C34A 120.0 . . ?
C36A C35A H35A 120.0 . . ?
C31A C36A H36A 120.0 . . ?
C35A C36A C31A 120.0 . . ?
C35A C36A H36A 120.0 . . ?
C32B C31B H31B 120.0 . . ?
C32B C31B C36B 120.0 . . ?
C36B C31B H31B 120.0 . . ?
C31B C32B H32B 120.0 . . ?
C33B C32B C31B 120.0 . . ?
C33B C32B H32B 120.0 . . ?
C32B C33B H33B 120.0 . . ?
C34B C33B C32B 120.0 . . ?
C34B C33B H33B 120.0 . . ?
C33B C34B H34B 120.0 . . ?
C35B C34B C33B 120.0 . . ?
C35B C34B H34B 120.0 . . ?
C34B C35B H35B 120.0 . . ?
C34B C35B C36B 120.0 . . ?
C36B C35B H35B 120.0 . . ?
C31B C36B H36B 120.0 . . ?
C35B C36B C31B 120.0 . . ?
C35B C36B H36B 120.0 . . ?
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
V1 Cl1 2.2040(6) . ?
V1 Cl2 2.2090(6) . ?
V1 Cl3 2.2073(6) . ?
V1 C6 1.706(2) . ?
N1 C2 1.355(3) . ?
N1 C5 1.379(3) . ?
N1 C7 1.445(3) . ?
N2 C2 1.358(3) . ?
N2 C4 1.376(3) . ?
N2 C19 1.447(3) . ?
C2 C6 1.412(3) . ?
C4 H4 0.9500 . ?
C4 C5 1.355(3) . ?
C5 H5 0.9500 . ?
C7 C8 1.398(3) . ?
C7 C12 1.400(3) . ?
C8 C9 1.394(3) . ?
C8 C13 1.521(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.382(4) . ?
C10 H10 0.9500 . ?
C10 C11 1.366(4) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(4) . ?
C12 C16 1.514(4) . ?
C13 H13 1.0000 . ?
C13 C14 1.525(4) . ?
C13 C15 1.528(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 1.0000 . ?
C16 C17 1.524(4) . ?
C16 C18 1.520(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C20 1.396(3) . ?
C19 C24 1.399(3) . ?
C20 C21 1.389(3) . ?
C20 C25 1.519(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.383(4) . ?
C22 H22 0.9500 . ?
C22 C23 1.377(4) . ?
C23 H23 0.9500 . ?
C23 C24 1.390(3) . ?
C24 C28 1.521(3) . ?
C25 H25 1.0000 . ?
C25 C26 1.513(4) . ?
C25 C27 1.521(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28 1.0000 . ?
C28 C29 1.527(3) . ?
C28 C30 1.523(4) . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31A H31A 0.9500 . ?
C31A C32A 1.3900 . ?
C31A C36A 1.3900 . ?
C32A H32A 0.9500 . ?
C32A C33A 1.3900 . ?
C33A H33A 0.9500 . ?
C33A C34A 1.3900 . ?
C34A H34A 0.9500 . ?
C34A C35A 1.3900 . ?
C35A H35A 0.9500 . ?
C35A C36A 1.3900 . ?
C36A H36A 0.9500 . ?
C31B H31B 0.9500 . ?
C31B C32B 1.3900 . ?
C31B C36B 1.3900 . ?
C32B H32B 0.9500 . ?
C32B C33B 1.3900 . ?
C33B H33B 0.9500 . ?
C33B C34B 1.3900 . ?
C34B H34B 0.9500 . ?
C34B C35B 1.3900 . ?
C35B H35B 0.9500 . ?
C35B C36B 1.3900 . ?
C36B H36B 0.9500 . ?
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
N1 C7 C8 C9 -177.6(2) . . . . ?
N1 C7 C8 C13 4.4(3) . . . . ?
N1 C7 C12 C11 177.4(2) . . . . ?
N1 C7 C12 C16 -0.9(3) . . . . ?
N2 C4 C5 N1 -0.1(3) . . . . ?
N2 C19 C20 C21 177.85(19) . . . . ?
N2 C19 C20 C25 -0.8(3) . . . . ?
N2 C19 C24 C23 -176.92(19) . . . . ?
N2 C19 C24 C28 3.1(3) . . . . ?
C2 N1 C5 C4 -0.4(3) . . . . ?
C2 N1 C7 C8 80.2(3) . . . . ?
C2 N1 C7 C12 -98.6(3) . . . . ?
C2 N2 C4 C5 0.5(3) . . . . ?
C2 N2 C19 C20 -94.6(3) . . . . ?
C2 N2 C19 C24 86.1(3) . . . . ?
C4 N2 C2 N1 -0.8(2) . . . . ?
C4 N2 C2 C6 179.4(2) . . . . ?
C4 N2 C19 C20 86.7(3) . . . . ?
C4 N2 C19 C24 -92.6(3) . . . . ?
C5 N1 C2 N2 0.7(2) . . . . ?
C5 N1 C2 C6 -179.4(2) . . . . ?
C5 N1 C7 C8 -99.5(3) . . . . ?
C5 N1 C7 C12 81.6(3) . . . . ?
C7 N1 C2 N2 -179.10(18) . . . . ?
C7 N1 C2 C6 0.8(3) . . . . ?
C7 N1 C5 C4 179.4(2) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C7 C8 C13 C14 84.5(3) . . . . ?
C7 C8 C13 C15 -152.5(2) . . . . ?
C7 C12 C16 C17 -134.1(3) . . . . ?
C7 C12 C16 C18 102.5(3) . . . . ?
C8 C7 C12 C11 -1.3(3) . . . . ?
C8 C7 C12 C16 -179.7(2) . . . . ?
C8 C9 C10 C11 -0.6(4) . . . . ?
C9 C8 C13 C14 -93.3(3) . . . . ?
C9 C8 C13 C15 29.7(3) . . . . ?
C9 C10 C11 C12 0.4(4) . . . . ?
C10 C11 C12 C7 0.5(4) . . . . ?
C10 C11 C12 C16 178.9(3) . . . . ?
C11 C12 C16 C17 47.6(3) . . . . ?
C11 C12 C16 C18 -75.8(3) . . . . ?
C12 C7 C8 C9 1.2(3) . . . . ?
C12 C7 C8 C13 -176.8(2) . . . . ?
C13 C8 C9 C10 177.8(2) . . . . ?
C19 N2 C2 N1 -179.67(19) . . . . ?
C19 N2 C2 C6 0.4(3) . . . . ?
C19 N2 C4 C5 179.4(2) . . . . ?
C19 C20 C21 C22 0.3(4) . . . . ?
C19 C20 C25 C26 98.4(3) . . . . ?
C19 C20 C25 C27 -136.8(3) . . . . ?
C19 C24 C28 C29 125.9(2) . . . . ?
C19 C24 C28 C30 -112.0(3) . . . . ?
C20 C19 C24 C23 3.8(3) . . . . ?
C20 C19 C24 C28 -176.2(2) . . . . ?
C20 C21 C22 C23 1.2(4) . . . . ?
C21 C20 C25 C26 -80.2(3) . . . . ?
C21 C20 C25 C27 44.6(3) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C22 C23 C24 C19 -2.2(3) . . . . ?
C22 C23 C24 C28 177.8(2) . . . . ?
C23 C24 C28 C29 -54.1(3) . . . . ?
C23 C24 C28 C30 68.1(3) . . . . ?
C24 C19 C20 C21 -2.9(3) . . . . ?
C24 C19 C20 C25 178.4(2) . . . . ?
C25 C20 C21 C22 179.0(2) . . . . ?
C31A C32A C33A C34A 0.0 . . . . ?
C32A C31A C36A C35A 0.0 . . . . ?
C32A C33A C34A C35A 0.0 . . . . ?
C33A C34A C35A C36A 0.0 . . . . ?
C34A C35A C36A C31A 0.0 . . . . ?
C36A C31A C32A C33A 0.0 . . . . ?
C31B C32B C33B C34B 0.0 . . . . ?
C32B C31B C36B C35B 0.0 . . . . ?
C32B C33B C34B C35B 0.0 . . . . ?
C33B C34B C35B C36B 0.0 . . . . ?
C34B C35B C36B C31B 0.0 . . . . ?
C36B C31B C32B C33B 0.0 . . . . ?
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 -0.0000 -0.9999 0.0238 -0.0989 0.0219
-1.0000 0.0000 0.9999 -0.0238 0.0989 -0.0219
0.0000 1.0000 -0.0001 -0.0838 0.0113 0.1426
-0.0000 -1.0000 0.0001 0.0838 -0.0113 -0.1426
-1.0000 0.0000 -0.0001 0.0357 0.0862 0.0141
0.9999 -2.0000 2.0002 0.0129 -0.0835 -0.3713
2.0000 -0.0000 -0.9999 -0.0118 -0.1851 0.0078
1.0000 0.0000 2.0000 -0.1546 -0.0609 -0.0861
-1.0000 -0.0000 -2.0000 0.1546 0.0609 0.0861
