# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_11054
_database_code_depnum_ccdc_archive 'CCDC 2055429'
loop_
_audit_author_name
_audit_author_address
'Qingrong Kong'
;Xiamen university
China
;
_audit_update_record             
;
2021-01-12 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_audit_creation_date             2020-06-20
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 O V, 2(C5 H13 Cl N)'
_chemical_formula_sum            'C10 H26 Cl6 N2 O V'
_chemical_formula_weight         453.97
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C10 N2 Cl6 V O'
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'
O O 0.0492 0.0322 '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'

_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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.75140(10)
_cell_length_b                   9.04080(10)
_cell_length_c                   12.5409(2)
_cell_angle_alpha                90
_cell_angle_beta                 95.9650(10)
_cell_angle_gamma                90
_cell_volume                     986.86(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8654
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      75.4700
_cell_measurement_theta_min      3.5450
_shelx_estimated_absorpt_T_max   0.204
_shelx_estimated_absorpt_T_min   0.128
_exptl_absorpt_coefficient_mu    11.654
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72125
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13844
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.615
_diffrn_reflns_theta_min         3.544
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4741
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -55.00 -11.00   1.00    1.00    --  -41.00 -57.00-120.00   44
  2  ω    -83.00 -13.00   1.00    1.00    --  -41.00 125.00  90.00   70
  3  ω    -38.00  -7.00   1.00    1.00    --  -41.00 -77.00 -60.00   31
  4  ω    -43.00  -7.00   1.00    1.00    --  -41.00 -77.00-180.00   36
  5  ω   -119.00 -23.00   1.00    1.00    --  -41.00 -77.00 150.00   96
  6  ω    -69.00  25.00   1.00    1.00    --  -41.00  57.00 -90.00   94
  7  ω   -118.00 -65.00   1.00    1.00    --  -41.00 -77.00   0.00   53
  8  ω    -47.00 -19.00   1.00    1.00    --  -41.00 -77.00   0.00   28
  9  ω   -115.00 -89.00   1.00    1.00    --  -41.00 -57.00-120.00   26
 10  ω   -117.00 -74.00   1.00    1.00    --  -41.00 -77.00 -60.00   43
 11  ω   -119.00  -8.00   1.00    1.00    --  -41.00 -77.00  60.00  111
 12  ω     15.00  42.00   1.00    1.00    --   41.00  57.00 -60.00   27
 13  ω     53.00  83.00   1.00    1.00    --   41.00 -99.00 -90.00   30
 14  ω    -29.00  67.00   1.00    1.00    --   41.00 -57.00   0.00   96
 15  ω     57.00  82.00   1.00    1.00    --   41.00  57.00 -60.00   25
 16  ω     81.00 108.00   1.00    3.00    --  111.51  61.00 120.00   27
 17  ω     81.00 140.00   1.00    3.00    --  111.51  61.00-150.00   59
 18  ω     81.00 120.00   1.00    3.00    --  111.51  61.00 -60.00   39
 19  ω     81.00 117.00   1.00    3.00    --  111.51  61.00  30.00   36
 20  ω     81.00 106.00   1.00    3.00    --  111.51  61.00 -90.00   25
 21  ω     38.00 116.00   1.00    3.00    --  111.51-125.00  30.00   78
 22  ω    139.00 177.00   1.00    3.00    --  111.51  61.00-107.31   38
 23  ω     78.00 165.00   1.00    3.00    --  111.51  77.00 150.00   87
 24  ω     82.00 178.00   1.00    3.00    --  111.51  61.00   0.00   96
 25  ω    148.00 174.00   1.00    3.00    --  111.51  61.00 -90.00   26
 26  ω     78.00 133.00   1.00    3.00    --  111.51  77.00  30.00   55
 27  ω     79.00 105.00   1.00    3.00    --  111.51  77.00-180.00   26
 28  ω     81.00 108.00   1.00    3.00    --  111.51  61.00 -30.00   27
 29  ω     27.00  92.00   1.00    3.00    --  111.51 -94.00 -90.00   65
 30  ω     78.00 111.00   1.00    3.00    --  111.51  77.00 -90.00   33
 31  ω     78.00 103.00   1.00    3.00    --  111.51  77.00  60.00   25
 32  ω     78.00 170.00   1.00    3.00    --  111.51  77.00-150.00   92
 33  ω     87.00 113.00   1.00    3.00    --  111.51  45.00   0.00   26
 34  ω     81.00 107.00   1.00    3.00    --  111.51  61.00 150.00   26
 35  ω     33.00 139.00   1.00    3.00    --  111.51 -77.00  30.00  106
 36  ω     79.00 104.00   1.00    3.00    --  111.51  77.00   0.00   25
 37  ω     78.00 175.00   1.00    3.00    --  111.51  77.00 -60.00   97
 38  ω     81.00 127.00   1.00    3.00    --  111.51  61.00  90.00   46
 39  ω    115.00 177.00   1.00    3.00    --  111.51  77.00  90.00   62
 40  ω     81.00 176.00   1.00    3.00    --  111.51  61.00  60.00   95
 41  ω     82.00 108.00   1.00    3.00    --  111.51  61.00-180.00   26
 42  ω     81.00 176.00   1.00    3.00    --  111.51  61.00-120.00   95
 43  ω     78.00 103.00   1.00    3.00    --  111.51  77.00  90.00   25
 44  ω     37.00 118.00   1.00    3.00    --  111.51-125.00-120.00   81
 45  ω     81.00 106.00   1.00    3.00    --  111.51  61.00-107.31   25
 46  ω     84.00 144.00   1.00    3.00    --  111.51  47.00 150.29   60
;
_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      -0.1448732000
_diffrn_orient_matrix_UB_12      -0.0297987000
_diffrn_orient_matrix_UB_13      -0.0777847000
_diffrn_orient_matrix_UB_21      -0.0440882000
_diffrn_orient_matrix_UB_22      -0.1278636000
_diffrn_orient_matrix_UB_23      0.0720529000
_diffrn_orient_matrix_UB_31      -0.0917074000
_diffrn_orient_matrix_UB_32      0.1085760000
_diffrn_orient_matrix_UB_33      0.0633488000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3863
_reflns_number_total             4026
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.271(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4026
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0423
_refine_ls_restrained_S_all      1.056
_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)+(0.0691P)²+0.6454P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1124
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.729(13)
 0.271(13)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C6(H6a,H6b), C9(H9a,H9b), C00K(H00a,H00b)
3.b Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C7(H7a,
 H7b,H7c), C8(H8a,H8b,H8c)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
V1 V 1.27988(9) 0.51615(9) 0.24092(6) 0.0213(2) Uani 1 1 d . . . . .
Cl1 Cl 1.07032(15) 0.67768(15) 0.20077(11) 0.0320(3) Uani 1 1 d . . . . .
Cl2 Cl 1.24815(16) 0.44861(16) 0.06084(10) 0.0338(3) Uani 1 1 d . . . . .
Cl3 Cl 0.73902(16) 0.83664(16) 0.31702(11) 0.0353(3) Uani 1 1 d . . . . .
Cl4 Cl 1.19440(19) 0.48643(19) 0.41007(11) 0.0458(4) Uani 1 1 d . . . . .
Cl5 Cl 1.4153(2) 0.29145(17) 0.27341(13) 0.0443(4) Uani 1 1 d . . . . .
Cl6 Cl 0.8456(2) 0.16365(19) 0.20685(13) 0.0473(4) Uani 1 1 d . . . . .
N1 N 0.7391(5) 0.4839(5) 0.5190(4) 0.0272(9) Uani 1 1 d . . . . .
O1 O 1.4181(5) 0.6313(5) 0.2540(4) 0.0389(10) Uani 1 1 d . . . . .
N2 N 0.7106(6) 0.4790(5) -0.0134(4) 0.0318(10) Uani 1 1 d . . . . .
C1 C 0.6909(6) 0.6218(6) 0.4559(5) 0.0284(11) Uani 1 1 d . . . . .
H1A H 0.6057 0.5974 0.4031 0.034 Uiso 1 1 calc R . . . .
H1B H 0.6548 0.6946 0.5043 0.034 Uiso 1 1 calc R . . . .
C2 C 0.8672(7) 0.5149(8) 0.6027(5) 0.0360(12) Uani 1 1 d . . . . .
H2A H 0.9574 0.5407 0.5694 0.054 Uiso 1 1 calc GR . . . .
H2B H 0.8876 0.4285 0.6464 0.054 Uiso 1 1 calc GR . . . .
H2C H 0.8395 0.5955 0.6467 0.054 Uiso 1 1 calc GR . . . .
C3 C 0.6629(8) 0.6004(7) 0.0561(6) 0.0386(14) Uani 1 1 d . . . . .
H3A H 0.7475 0.6267 0.1076 0.058 Uiso 1 1 calc GR . . . .
H3B H 0.5781 0.5679 0.0928 0.058 Uiso 1 1 calc GR . . . .
H3C H 0.6325 0.6849 0.0127 0.058 Uiso 1 1 calc GR . . . .
C4 C 0.6014(7) 0.4361(8) 0.5723(6) 0.0390(14) Uani 1 1 d . . . . .
H4A H 0.5753 0.5117 0.6210 0.059 Uiso 1 1 calc GR . . . .
H4B H 0.6246 0.3459 0.6111 0.059 Uiso 1 1 calc GR . . . .
H4C H 0.5163 0.4200 0.5188 0.059 Uiso 1 1 calc GR . . . .
C5 C 0.8511(7) 0.5241(8) -0.0614(5) 0.0400(13) Uani 1 1 d . . . . .
H5A H 0.8285 0.6078 -0.1075 0.060 Uiso 1 1 calc GR . . . .
H5B H 0.8861 0.4435 -0.1024 0.060 Uiso 1 1 calc GR . . . .
H5C H 0.9298 0.5502 -0.0055 0.060 Uiso 1 1 calc GR . . . .
C6 C 0.8184(8) 0.6893(8) 0.3994(6) 0.0394(14) Uani 1 1 d . . . . .
H6A H 0.8626 0.6152 0.3557 0.047 Uiso 1 1 calc R . . . .
H6B H 0.8988 0.7265 0.4515 0.047 Uiso 1 1 calc R . . . .
C7 C 0.5844(9) 0.4513(9) -0.1012(5) 0.0452(15) Uani 1 1 d . . . . .
H7A H 0.4915 0.4271 -0.0705 0.068 Uiso 1 1 calc GR . . . .
H7B H 0.6125 0.3706 -0.1449 0.068 Uiso 1 1 calc GR . . . .
H7C H 0.5681 0.5386 -0.1445 0.068 Uiso 1 1 calc GR . . . .
C8 C 0.7829(9) 0.3614(7) 0.4479(6) 0.0417(15) Uani 1 1 d . . . . .
H8A H 0.7055 0.3509 0.3883 0.063 Uiso 1 1 calc GR . . . .
H8B H 0.7915 0.2706 0.4878 0.063 Uiso 1 1 calc GR . . . .
H8C H 0.8797 0.3839 0.4221 0.063 Uiso 1 1 calc GR . . . .
C9 C 0.7227(9) 0.3328(8) 0.0482(6) 0.0436(15) Uani 1 1 d . . . . .
H9A H 0.6269 0.3143 0.0784 0.052 Uiso 1 1 calc R . . . .
H9B H 0.7386 0.2529 -0.0011 0.052 Uiso 1 1 calc R . . . .
C00K C 0.8523(11) 0.3340(11) 0.1366(8) 0.064(2) Uani 1 1 d . . . . .
H00A H 0.8408 0.4164 0.1847 0.077 Uiso 1 1 calc R . . . .
H00B H 0.9499 0.3441 0.1071 0.077 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
V1 Cl1 2.3575(15) . ?
V1 Cl2 2.3280(14) . ?
V1 Cl4 2.3370(16) . ?
V1 Cl5 2.3657(16) . ?
V1 O1 1.591(4) . ?
Cl3 C6 1.782(6) . ?
Cl6 C00K 1.779(9) . ?
N1 C1 1.513(7) . ?
N1 C2 1.481(7) . ?
N1 C4 1.501(7) . ?
N1 C8 1.496(8) . ?
N2 C3 1.487(7) . ?
N2 C5 1.481(8) . ?
N2 C7 1.498(8) . ?
N2 C9 1.529(8) . ?
C1 C6 1.512(8) . ?
C9 C00K 1.501(11) . ?

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 Cl5 158.96(7) . . ?
Cl2 V1 Cl1 86.77(5) . . ?
Cl2 V1 Cl4 146.43(7) . . ?
Cl2 V1 Cl5 87.07(6) . . ?
Cl4 V1 Cl1 87.12(6) . . ?
Cl4 V1 Cl5 86.95(6) . . ?
O1 V1 Cl1 100.52(19) . . ?
O1 V1 Cl2 106.52(18) . . ?
O1 V1 Cl4 107.06(18) . . ?
O1 V1 Cl5 100.52(18) . . ?
C2 N1 C1 111.4(4) . . ?
C2 N1 C4 108.8(5) . . ?
C2 N1 C8 109.9(5) . . ?
C4 N1 C1 106.1(4) . . ?
C8 N1 C1 111.9(5) . . ?
C8 N1 C4 108.6(5) . . ?
C3 N2 C7 108.9(5) . . ?
C3 N2 C9 110.6(5) . . ?
C5 N2 C3 109.3(5) . . ?
C5 N2 C7 109.1(5) . . ?
C5 N2 C9 115.2(5) . . ?
C7 N2 C9 103.5(5) . . ?
C6 C1 N1 113.5(5) . . ?
C1 C6 Cl3 108.1(4) . . ?
C00K C9 N2 112.0(6) . . ?
C9 C00K Cl6 107.4(6) . . ?

_olex2_date_sample_data_collection 2020-06-07
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.448
_oxdiff_exptl_absorpt_empirical_full_min 0.733
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.729(13)
2 0.271(13)

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_8741
_database_code_depnum_ccdc_archive 'CCDC 2055430'
loop_
_audit_author_name
_audit_author_address
'Qingrong Kong'
;Xiamen university
China
;
_audit_update_record             
;
2021-01-12 deposited with the CCDC.	2021-06-16 downloaded from the CCDC.
;
_audit_creation_date             2020-11-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'Cl4 O V, 2(C5 H13 Cl N)'
_chemical_formula_sum            'C10 H26 Cl6 N2 O V'
_chemical_formula_weight         453.97
_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 0.0181 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'
O O 0.0492 0.0322 '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'

_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/n 1'
_space_group_name_Hall           '-P 2yn'
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'

_cell_length_a                   8.7533(4)
_cell_length_b                   9.0953(4)
_cell_length_c                   12.7626(6)
_cell_angle_alpha                90
_cell_angle_beta                 95.135(4)
_cell_angle_gamma                90
_cell_volume                     1012.00(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4871
_cell_measurement_temperature    300.00(11)
_cell_measurement_theta_max      73.7250
_cell_measurement_theta_min      4.8390
_shelx_estimated_absorpt_T_max   0.342
_shelx_estimated_absorpt_T_min   0.210
_exptl_absorpt_coefficient_mu    11.365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10601
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.061
_diffrn_reflns_theta_min         5.892
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     25.00  72.00   0.50    0.31    --   43.22-105.00 -78.00   94
  2  ω     36.00  62.00   0.50    0.31    --   43.22 -99.00   0.00   52
  3  ω     65.00 110.00   0.50    1.24    --  107.45-105.00 -78.00   90
  4  ω     55.00  81.00   0.50    1.24    --  107.45 -94.00  30.00   52
  5  ω     33.00  62.00   0.50    1.24    --  107.45-105.00 -78.00   58
  6  ω     33.00 100.00   0.50    1.24    --  107.45 -94.00 120.00  134
  7  ω     91.00 116.00   0.50    1.24    --  107.45-125.00 120.00   50
  8  ω     33.00  85.00   0.50    1.24    --  107.45-125.00 120.00  104
  9  ω     89.00 123.00   0.50    1.24    --  107.45  77.00  90.00   68
 10  ω    138.00 178.00   0.50    1.24    --  107.45  77.00  90.00   80
 11  ω    149.00 178.00   0.50    1.24    --  107.45 125.00 120.00   58
 12  ω    106.00 132.00   0.50    1.24    --  107.45 105.00  22.00   52
 13  ω     93.00 174.00   0.50    1.24    --  107.45 125.00 -30.00  162
 14  ω    107.00 133.00   0.50    1.24    --  107.45 125.00 120.00   52
 15  ω    -63.00 -31.00   0.50    1.24    --  -90.25 105.00  22.00   64
 16  ω    -85.00 -22.00   0.50    0.31    --  -43.22 105.00  22.00  126
 17  ω   -108.00 -74.00   0.50    0.31    --  -43.22-125.00 -60.00   68
 18  ω   -116.00 -73.00   0.50    0.31    --  -43.22-125.00-120.00   86
 19  ω   -122.00 -81.00   0.50    1.24    --  -90.25-105.00 -78.00   82
 20  ω   -115.00 -70.00   0.50    0.31    --  -43.22-125.00   0.00   90
 21  ω   -113.00 -74.00   0.50    0.31    --  -43.22-125.00  60.00   78
 22  ω   -115.00 -74.00   0.50    0.31    --  -43.22-125.00  90.00   82
 23  ω   -134.00 -94.00   0.50    1.24    --  -90.25 -94.00  30.00   80
 24  ω   -159.00 -72.00   0.50    1.24    --  -90.25 -45.00 120.00  174
 25  ω    -18.00   8.00   0.50    0.30    --  -43.22 103.00  25.00   52
 26  ω   -118.00 -67.00   0.50    0.30    --  -43.22 -57.00-180.00  102
 27  ω    -62.00 -20.00   0.50    0.30    --  -43.22 -57.00-180.00   84
 28  ω     38.00  84.00   0.50    0.30    --   43.22-125.00-120.00   92
 29  ω      4.00  31.00   0.50    0.30    --   43.22 -99.00 -90.00   54
 30  ω    -87.00 -52.00   0.50    0.20    --  -90.25 125.00  30.00   70
 31  ω    -43.00 -17.00   0.50    0.20    --  -90.25 125.00  90.00   52
 32  ω    -46.00 -16.00   0.50    0.20    --  -90.25 125.00  30.00   60
 33  ω   -113.00 -23.00   0.50    0.20    --  -90.25  45.00  60.00  180
 34  ω     35.00  79.00   0.50    0.20    --  107.45-125.00 -90.00   88
 35  ω    146.00 176.00   0.50    0.20    --  107.45  45.00 150.00   60
 36  ω     94.00 136.00   0.50    0.20    --  107.45 -77.00 150.00   84
 37  ω    103.00 128.00   0.50    0.20    --  107.45  45.00 150.00   50
 38  ω    131.00 178.00   0.50    0.20    --  107.45  61.00  60.00   94
 39  ω     83.00 112.00   0.50    0.20    --  107.45-125.00 -90.00   58
 40  ω     92.00 117.00   0.50    0.20    --  107.45-125.00  60.00   50
 41  ω     35.00  61.00   0.50    0.20    --  107.45-125.00  60.00   52
 42  ω     36.00  90.00   0.50    0.20    --  107.45-125.00-180.00  108
 43  ω     54.00  79.00   0.50    0.20    --  107.45 -94.00 -60.00   50
 44  ω     93.00 119.00   0.50    0.20    --  107.45  61.00  60.00   52
 45  ω     38.00  65.00   0.50    0.20    --  107.45 -77.00 150.00   54
 46  ω    116.00 141.00   0.50    0.20    --  107.45 103.00  25.00   50
 47  ω    -62.00 -37.00   0.50    0.30    --  -43.22 103.00  25.00   50
 48  ω     46.00  71.00   0.50    0.20    --  107.45-103.00 -77.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0396035000
_diffrn_orient_matrix_UB_12      0.1461190000
_diffrn_orient_matrix_UB_13      0.0573178000
_diffrn_orient_matrix_UB_21      -0.0345788000
_diffrn_orient_matrix_UB_22      -0.0705459000
_diffrn_orient_matrix_UB_23      0.1050683000
_diffrn_orient_matrix_UB_31      0.1685923000
_diffrn_orient_matrix_UB_32      -0.0486255000
_diffrn_orient_matrix_UB_33      0.0195583000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1635
_reflns_number_total             2013
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.082
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         2013
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0758
_refine_ls_restrained_S_all      1.131
_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)+(0.1063P)²+1.3623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2182
_refine_ls_wR_factor_ref         0.2326
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(Cl4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=1-FVAR(1)
 Sof(Cl3)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
 Fixed Sof: O1(0.5) V1(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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
Cl1 Cl 0.6666(2) 0.69204(18) 0.53360(13) 0.1017(6) Uani 1 1 d . . . . .
Cl2 Cl 0.4822(2) 0.4754(2) 0.67649(12) 0.1024(6) Uani 1 1 d . . . . .
Cl3 Cl 0.0190(9) 0.8475(6) 0.4353(5) 0.0852(13) Uani 0.56(2) 1 d . . P A 1
N1 N -0.0118(5) 0.5015(4) 0.2357(3) 0.0703(11) Uani 1 1 d . . . . .
C1 C -0.1370(7) 0.5353(7) 0.1545(5) 0.0878(16) Uani 1 1 d . . . . .
H1A H -0.1082 0.6174 0.1133 0.132 Uiso 1 1 calc GR . . . .
H1B H -0.2281 0.5592 0.1876 0.132 Uiso 1 1 calc GR . . . .
H1C H -0.1562 0.4513 0.1097 0.132 Uiso 1 1 calc GR . . . .
C2 C 0.1263(8) 0.4557(8) 0.1822(6) 0.0953(18) Uani 1 1 d . . . . .
H2A H 0.1013 0.3714 0.1387 0.143 Uiso 1 1 calc GR . . . .
H2B H 0.2085 0.4313 0.2342 0.143 Uiso 1 1 calc GR . . . .
H2C H 0.1577 0.5350 0.1393 0.143 Uiso 1 1 calc GR . . . .
C3 C -0.0572(10) 0.3802(7) 0.3038(6) 0.108(2) Uani 1 1 d . . . . .
H3A H -0.1507 0.4058 0.3333 0.162 Uiso 1 1 calc GR . . . .
H3B H 0.0223 0.3641 0.3594 0.162 Uiso 1 1 calc GR . . . .
H3C H -0.0726 0.2922 0.2627 0.162 Uiso 1 1 calc GR . . . .
C4 C 0.0640(14) 0.6350(12) 0.2953(8) 0.061(3) Uani 0.56(2) 1 d . . P A 1
H4A H 0.1540 0.6038 0.3395 0.073 Uiso 0.56(2) 1 calc R . P A 1
H4B H 0.0951 0.7076 0.2457 0.073 Uiso 0.56(2) 1 calc R . P A 1
O1 O 0.3283(9) 0.6374(10) 0.4984(7) 0.093(2) Uani 0.5 1 d . . P . .
C5 C -0.0550(14) 0.7002(14) 0.3623(10) 0.090(4) Uani 0.56(2) 1 d . . P A 1
H5A H -0.0884 0.6252 0.4093 0.108 Uiso 0.56(2) 1 calc R . P A 1
H5B H -0.1437 0.7321 0.3170 0.108 Uiso 0.56(2) 1 calc R . P A 1
V1 V 0.53132(15) 0.47296(15) 0.49481(12) 0.0492(4) Uani 0.5 1 d . . P . .
Cl4 Cl 0.0828(18) 0.8175(12) 0.4531(6) 0.097(3) Uani 0.44(2) 1 d . . P A 2
C6 C 0.088(3) 0.658(3) 0.385(2) 0.161(12) Uani 0.44(2) 1 d . . P A 2
H6A H 0.1881 0.6469 0.3592 0.193 Uiso 0.44(2) 1 calc R . P A 2
H6B H 0.0732 0.5762 0.4319 0.193 Uiso 0.44(2) 1 calc R . P A 2
C7 C -0.022(3) 0.6489(19) 0.3006(15) 0.092(5) Uani 0.44(2) 1 d . . P A 2
H7A H -0.0096 0.7318 0.2543 0.111 Uiso 0.44(2) 1 calc R . P A 2
H7B H -0.1225 0.6560 0.3261 0.111 Uiso 0.44(2) 1 calc R . P A 2


_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
Cl1 V1 2.296(2) 3_666 ?
Cl1 V1 2.348(2) . ?
Cl2 V1 2.229(2) 3_666 ?
Cl2 V1 2.396(2) . ?
Cl3 C5 1.725(13) . ?
N1 C1 1.471(8) . ?
N1 C2 1.500(8) . ?
N1 C3 1.480(8) . ?
N1 C4 1.549(11) . ?
N1 C7 1.582(18) . ?
C4 C5 1.526(16) . ?
O1 V1 2.327(7) . ?
O1 V1 1.584(7) 3_666 ?
V1 Cl1 2.296(2) 3_666 ?
V1 Cl2 2.229(2) 3_666 ?
V1 O1 1.584(7) 3_666 ?
V1 V1 0.757(2) 3_666 ?
Cl4 C6 1.70(2) . ?
C6 C7 1.37(3) . ?

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
V1 Cl1 V1 18.72(5) 3_666 . ?
V1 Cl2 V1 18.39(6) 3_666 . ?
C1 N1 C2 108.5(5) . . ?
C1 N1 C3 110.3(5) . . ?
C1 N1 C4 116.2(6) . . ?
C1 N1 C7 96.9(9) . . ?
C2 N1 C4 96.5(6) . . ?
C2 N1 C7 123.9(10) . . ?
C3 N1 C2 109.2(5) . . ?
C3 N1 C4 114.9(6) . . ?
C3 N1 C7 107.1(8) . . ?
C5 C4 N1 107.2(9) . . ?
V1 O1 V1 4.28(14) 3_666 . ?
C4 C5 Cl3 111.3(8) . . ?
Cl1 V1 Cl1 161.28(5) 3_666 . ?
Cl1 V1 Cl2 85.35(7) . . ?
Cl1 V1 Cl2 87.74(8) 3_666 . ?
Cl1 V1 O1 81.8(3) 3_666 . ?
Cl2 V1 Cl1 90.54(8) 3_666 . ?
Cl2 V1 Cl1 90.56(8) 3_666 3_666 ?
Cl2 V1 Cl2 161.61(6) 3_666 . ?
Cl2 V1 O1 84.9(2) 3_666 . ?
O1 V1 Cl1 79.7(2) . . ?
O1 V1 Cl1 99.5(4) 3_666 3_666 ?
O1 V1 Cl1 98.8(4) 3_666 . ?
O1 V1 Cl2 99.1(3) 3_666 . ?
O1 V1 Cl2 99.2(3) 3_666 3_666 ?
O1 V1 Cl2 76.8(2) . . ?
O1 V1 O1 175.72(14) 3_666 . ?
V1 V1 Cl1 76.8(2) 3_666 . ?
V1 V1 Cl1 84.5(2) 3_666 3_666 ?
V1 V1 Cl2 93.4(2) 3_666 3_666 ?
V1 V1 Cl2 68.2(2) 3_666 . ?
V1 V1 O1 9.0(3) 3_666 . ?
V1 V1 O1 166.7(4) 3_666 3_666 ?
C7 C6 Cl4 114(2) . . ?
C6 C7 N1 113.0(19) . . ?

_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 3.337
_oxdiff_exptl_absorpt_empirical_full_min 0.628
