# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2023

####################################################################### 
# 
# 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_cl3nb-1
_database_code_depnum_ccdc_archive 'CCDC 2254035'
loop_
_audit_author_name
_audit_author_address
'Charlotte L. Stern'
;Northwestern University
United States of America
;
_audit_update_record             
;
2023-06-16 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_audit_creation_date             2023-06-15
_audit_creation_method           
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_shelx_SHELXL_version_number     2019/2
loop_
_audit_author_email
''
_chemical_name_common            ?
_chemical_name_systematic        
tetrachlorido-[1,2-bis(methoxy)ethane]-niobium
_chemical_formula_moiety         'C4 H10 Cl4 Nb O2'
_chemical_formula_sum            'C4 H10 Cl4 Nb O2'
_chemical_formula_weight         324.83
_chemical_absolute_configuration ad
_chemical_melting_point          ?
_chemical_oxdiff_formula         Cl3NbCNOH
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   8.11655(12)
_cell_length_b                   11.38883(17)
_cell_length_c                   11.79824(19)
_cell_angle_alpha                90
_cell_angle_beta                 90.2289(14)
_cell_angle_gamma                90
_cell_volume                     1090.60(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    25936
_cell_measurement_temperature    100.00(16)
_cell_measurement_theta_max      33.8290
_cell_measurement_theta_min      3.0580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.039
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.553
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             636
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.1313
0 1 0 0.0441
0 -1 0 0.0561
-1 -1 0 0.1139
0 0 1 0.0212
0 0 -1 0.0422

_exptl_crystal_recrystallization_method 
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.063
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
0.9991 0.0015 -0.0007 0.0209 0.0784 0.0323
-0.0005 0.9992 -0.0027 -0.0145 -0.0197 0.0572
0.0005 -0.9992 0.0027 0.0145 0.0197 -0.0572
-0.9986 -1.0007 0.0034 -0.0064 -0.0587 -0.0895
0.0002 0.0020 0.9986 0.0566 -0.0182 0.0081
-0.0002 -0.0020 -0.9986 -0.0566 0.0182 -0.0081

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.761
_diffrn_reflns_theta_min         3.082
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.959
_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 -30.00   0.50    2.33    --  -12.70 157.00  -0.00   98
  2  ω    -54.00  -8.00   0.50    2.33    --  -12.70 118.00-154.00   92
  3  ω     30.00  81.00   0.50    2.33    --   13.95-157.00 -35.00  102
  4  ω      8.00  55.00   0.50    2.33    --   13.95-118.00 119.00   94
  5  ω    -70.00 -21.00   0.50    2.33    --  -12.70 141.00 -85.22   98
  6  ω    -67.00 -19.00   0.50    2.33    --  -12.70 137.00  64.75   96
  7  ω    -85.00  10.00   0.50    2.33    --  -12.70 -77.00  60.00  190
  8  ω    -70.00 -21.00   0.50    2.33    --  -12.70 141.00 106.65   98
  9  ω    -70.00 -21.00   0.50    2.33    --  -12.70 141.00-118.75   98
 10  ω    -68.00 -20.00   0.50    2.33    --  -12.70 138.00 -50.50   96
 11  ω    -85.00  10.00   0.50    2.33    --  -12.70 -77.00-120.00  190
 12  ω    -42.00  42.00   0.50    2.33    --  -12.70  91.00  20.09  168
 13  ω    -86.00   0.00   0.50    2.33    --  -12.70 -37.00 -90.00  172
 14  ω      2.00  87.00   0.50    2.33    --   13.95  37.00-180.00  170
 15  ω     -9.00  87.00   0.50    2.33    --   13.95  77.00 -60.00  192
 16  ω    -60.00   5.00   0.50    2.33    --   13.95 -19.00 150.00  130
 17  ω      2.00  87.00   0.50    2.33    --   13.95  37.00 150.00  170
 18  ω    -41.00  44.00   0.50    2.33    --   13.95 -92.00-125.20  170
 19  ω    -60.00   5.00   0.50    2.33    --   13.95 -19.00 -30.00  130
 20  ω    -66.00 -18.00   0.50    2.33    --  -12.70 135.00-161.99   96
 21  ω    -70.00 -21.00   0.50    2.33    --  -12.70 141.00 -10.98   98
 22  ω    -24.00  21.00   0.50    2.33    --  -12.70 -99.00 150.00   90
 23  ω    -24.00  21.00   0.50    2.33    --  -12.70 -99.00-180.00   90
 24  ω    -69.00 -21.00   0.50    2.33    --  -12.70 140.00  86.48   96
 25  ω    -68.00 -20.00   0.50    2.33    --  -12.70 138.00 157.93   96
 26  ω    -66.00 -18.00   0.50    2.33    --  -12.70 135.00  43.90   96
 27  ω    -23.00  24.00   0.50    2.33    --   13.95 -99.00  60.00   94
 28  ω      2.00  87.00   0.50    2.33    --   13.95  37.00  90.00  170
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0209904000
_diffrn_orient_matrix_UB_12      -0.0143877000
_diffrn_orient_matrix_UB_13      0.0567454000
_diffrn_orient_matrix_UB_21      0.0784469000
_diffrn_orient_matrix_UB_22      -0.0197329000
_diffrn_orient_matrix_UB_23      -0.0181652000
_diffrn_orient_matrix_UB_31      0.0322826000
_diffrn_orient_matrix_UB_32      0.0572961000
_diffrn_orient_matrix_UB_33      0.0080111000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_reflns_Friedel_coverage         0.935
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                3985
_reflns_number_total             4052
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         3.201
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details 
;
 Flack x determined using 1883 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(4)
_refine_ls_extinction_coef       .
_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     103
_refine_ls_number_reflns         4052
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0418
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0868P)²+1.5585P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1122
_refine_special_details          
'The crystal under investigation was found to be pseudo-merohedrally twinned. The orientation matrices for the two components were identified using the program PLATON (A.L.Spek (2002)).  The twin fraction refined to a value of 0.168(2).'
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.833(2)
 0.167(2)
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), C2(H2A,H2B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_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
Nb1 Nb 0.57191(6) 0.76460(4) 0.50160(6) 0.01721(12) Uani 1 1 d . . . . .
Cl1 Cl 0.7249(3) 0.92211(17) 0.57746(17) 0.0344(4) Uani 1 1 d . . . . .
Cl2 Cl 0.8059(2) 0.65187(19) 0.45648(17) 0.0294(3) Uani 1 1 d . . . . .
Cl3 Cl 0.5361(2) 0.66734(13) 0.67637(12) 0.0223(3) Uani 1 1 d . . . . .
Cl4 Cl 0.5456(2) 0.85614(15) 0.32313(13) 0.0248(3) Uani 1 1 d . . . . .
O1 O 0.3287(7) 0.8364(4) 0.5416(4) 0.0222(9) Uani 1 1 d . . . . .
O2 O 0.4007(6) 0.6376(4) 0.4309(4) 0.0182(8) Uani 1 1 d . . . . .
C1 C 0.1966(9) 0.7529(7) 0.5224(8) 0.0265(15) Uani 1 1 d . . . . .
H1A H 0.090647 0.794914 0.513398 0.032 Uiso 1 1 calc R U . . .
H1B H 0.187446 0.699269 0.588156 0.032 Uiso 1 1 calc R U . . .
C2 C 0.2335(8) 0.6838(7) 0.4173(7) 0.0246(12) Uani 1 1 d . . . . .
H2A H 0.153610 0.618747 0.408287 0.030 Uiso 1 1 calc R U . . .
H2B H 0.226647 0.734939 0.349555 0.030 Uiso 1 1 calc R U . . .
C3 C 0.2987(14) 0.9082(8) 0.6399(7) 0.0371(18) Uani 1 1 d . . . . .
H3A H 0.303714 0.859250 0.708170 0.056 Uiso 1 1 calc R U . . .
H3B H 0.189420 0.944177 0.633723 0.056 Uiso 1 1 calc R U . . .
H3C H 0.382683 0.969823 0.644710 0.056 Uiso 1 1 calc R U . . .
C4 C 0.4394(9) 0.5525(6) 0.3444(6) 0.0263(13) Uani 1 1 d . . . . .
H4A H 0.429553 0.589320 0.269545 0.039 Uiso 1 1 calc R U . . .
H4B H 0.362539 0.486385 0.349363 0.039 Uiso 1 1 calc R U . . .
H4C H 0.552287 0.524148 0.355392 0.039 Uiso 1 1 calc R U . . .


_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
Nb1 Cl1 2.3565(18) . ?
Nb1 Cl2 2.3551(19) . ?
Nb1 Cl3 2.3596(15) . ?
Nb1 Cl4 2.3585(15) . ?
Nb1 O1 2.190(5) . ?
Nb1 O2 2.170(4) . ?
O1 C1 1.451(10) . ?
O1 C3 1.440(9) . ?
O2 C2 1.465(8) . ?
O2 C4 1.442(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1 C2 1.500(12) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Nb1 Cl3 95.28(6) . . ?
Cl1 Nb1 Cl4 92.76(6) . . ?
Cl2 Nb1 Cl1 94.39(9) . . ?
Cl2 Nb1 Cl3 92.52(7) . . ?
Cl2 Nb1 Cl4 96.27(7) . . ?
Cl4 Nb1 Cl3 167.59(6) . . ?
O1 Nb1 Cl1 96.20(16) . . ?
O1 Nb1 Cl2 168.74(15) . . ?
O1 Nb1 Cl3 82.70(14) . . ?
O1 Nb1 Cl4 87.06(14) . . ?
O2 Nb1 Cl1 171.54(14) . . ?
O2 Nb1 Cl2 93.74(14) . . ?
O2 Nb1 Cl3 86.68(14) . . ?
O2 Nb1 Cl4 84.03(14) . . ?
O2 Nb1 O1 75.86(19) . . ?
C1 O1 Nb1 112.8(4) . . ?
C3 O1 Nb1 122.7(6) . . ?
C3 O1 C1 111.7(6) . . ?
C2 O2 Nb1 113.2(4) . . ?
C4 O2 Nb1 125.4(4) . . ?
C4 O2 C2 111.6(5) . . ?
O1 C1 H1A 109.9 . . ?
O1 C1 H1B 109.9 . . ?
O1 C1 C2 108.9(6) . . ?
H1A C1 H1B 108.3 . . ?
C2 C1 H1A 109.9 . . ?
C2 C1 H1B 109.9 . . ?
O2 C2 C1 106.6(6) . . ?
O2 C2 H2A 110.4 . . ?
O2 C2 H2B 110.4 . . ?
C1 C2 H2A 110.4 . . ?
C1 C2 H2B 110.4 . . ?
H2A C2 H2B 108.6 . . ?
O1 C3 H3A 109.5 . . ?
O1 C3 H3B 109.5 . . ?
O1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
O2 C4 H4A 109.5 . . ?
O2 C4 H4B 109.5 . . ?
O2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
Nb1 O1 C1 C2 -38.6(7) . . . . ?
Nb1 O2 C2 C1 -42.4(6) . . . . ?
O1 C1 C2 O2 52.1(7) . . . . ?
C3 O1 C1 C2 178.4(6) . . . . ?
C4 O2 C2 C1 169.7(6) . . . . ?

_olex2_date_sample_data_collection 2023-04-11
_olex2_date_sample_submission    2023-04-11
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a MITIGEN holder in paratone oil'
_olex2_submission_original_sample_id NbCl4(dme)
_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 1.188
_oxdiff_exptl_absorpt_empirical_full_min 0.782
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.833(2)
2 0.167(2)

_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_288
_database_code_depnum_ccdc_archive 'CCDC 2254037'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2023-04-05 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_audit_creation_date             2021-12-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Tetrachlorobis(diethyl ether)tantalum(IV)'
_chemical_formula_moiety         'C8 H20 Cl4 O2 Ta'
_chemical_formula_sum            'C8 H20 Cl4 O2 Ta'
_chemical_formula_weight         470.99
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta Cl O C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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                   7.6010(3)
_cell_length_b                   11.3893(3)
_cell_length_c                   8.9865(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.050(4)
_cell_angle_gamma                90
_cell_volume                     743.77(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3257
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.4730
_cell_measurement_theta_min      2.9600
_shelx_estimated_absorpt_T_max   0.717
_shelx_estimated_absorpt_T_min   0.101
_exptl_absorpt_coefficient_mu    8.089
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50637
_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 bluish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             450
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.044
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6261
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.640
_diffrn_reflns_theta_min         2.970
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     24.00  53.00   0.50   30.00    --   20.00  54.00 -90.00   58
  2  ω     62.00 108.00   0.50   30.00    --   20.00  54.00 -90.00   92
  3  ω    -71.00  66.00   0.50   30.00    --   20.00  54.00 120.00  274
  4  ω    -74.00 -25.00   0.50   30.00    --   20.00  54.00 -30.00   98
  5  ω     28.00 107.00   0.50   30.00    --   20.00  54.00 -30.00  158
  6  ω    -66.00   9.00   0.50   30.00    --   20.00  54.00  60.00  150
  7  ω     42.00  67.00   0.50   30.00    --   20.00  54.00  60.00   50
  8  ω     82.00 107.00   0.50   30.00    --   20.00  54.00  60.00   50
  9  ω    -48.00 -23.00   0.50   30.00    --   20.00  54.00 -90.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0232848000
_diffrn_orient_matrix_UB_12      0.0294254000
_diffrn_orient_matrix_UB_13      -0.0611218000
_diffrn_orient_matrix_UB_21      -0.0527473000
_diffrn_orient_matrix_UB_22      0.0491725000
_diffrn_orient_matrix_UB_23      0.0096978000
_diffrn_orient_matrix_UB_31      0.0787635000
_diffrn_orient_matrix_UB_32      0.0242931000
_diffrn_orient_matrix_UB_33      0.0547829000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1872
_reflns_number_total             2188
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         1.545
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         2188
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0190
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0160P)²+0.3611P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0391
_refine_ls_wR_factor_ref         0.0409
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Ta1 Ta 0.500000 0.500000 0.500000 0.01028(4) Uani 1 2 d S . P . .
Cl3 Cl 0.49522(8) 0.63046(5) 0.29104(7) 0.01776(12) Uani 1 1 d . . . . .
Cl1 Cl 0.81702(8) 0.54046(6) 0.62444(7) 0.01820(12) Uani 1 1 d . . . . .
O1 O 0.4249(2) 0.64010(15) 0.62349(19) 0.0145(3) Uani 1 1 d . . . . .
C1 C 0.5152(3) 0.7562(2) 0.6438(3) 0.0173(5) Uani 1 1 d . . . . .
H1A H 0.619549 0.753502 0.602475 0.021 Uiso 1 1 calc R U . . .
H1B H 0.561250 0.773810 0.754015 0.021 Uiso 1 1 calc R U . . .
C2 C 0.2758(3) 0.6292(2) 0.6984(3) 0.0169(5) Uani 1 1 d . . . . .
H2A H 0.218468 0.552729 0.674304 0.020 Uiso 1 1 calc R U . . .
H2B H 0.182807 0.688279 0.655525 0.020 Uiso 1 1 calc R U . . .
C3 C 0.3870(4) 0.8527(2) 0.5636(3) 0.0228(6) Uani 1 1 d . . . . .
H3A H 0.338612 0.834754 0.454832 0.034 Uiso 1 1 calc R U . . .
H3B H 0.453062 0.925605 0.575999 0.034 Uiso 1 1 calc R U . . .
H3C H 0.287626 0.859218 0.608833 0.034 Uiso 1 1 calc R U . . .
C4 C 0.3449(4) 0.6438(2) 0.8723(3) 0.0235(6) Uani 1 1 d . . . . .
H4A H 0.380235 0.724028 0.896989 0.035 Uiso 1 1 calc R U . . .
H4B H 0.449335 0.593637 0.913669 0.035 Uiso 1 1 calc R U . . .
H4C H 0.249119 0.622975 0.917269 0.035 Uiso 1 1 calc R U . . .


_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
Ta1 Cl3 2.3865(6) 3_666 ?
Ta1 Cl3 2.3865(6) . ?
Ta1 Cl1 2.3852(6) . ?
Ta1 Cl1 2.3852(6) 3_666 ?
Ta1 O1 2.1153(17) 3_666 ?
Ta1 O1 2.1153(17) . ?
O1 C1 1.476(3) . ?
O1 C2 1.483(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C1 C3 1.505(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.505(3) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

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
Cl3 Ta1 Cl3 180.0 . 3_666 ?
Cl1 Ta1 Cl3 88.35(2) 3_666 . ?
Cl1 Ta1 Cl3 91.65(2) 3_666 3_666 ?
Cl1 Ta1 Cl3 88.35(2) . 3_666 ?
Cl1 Ta1 Cl3 91.65(2) . . ?
Cl1 Ta1 Cl1 180.0 3_666 . ?
O1 Ta1 Cl3 90.06(5) 3_666 . ?
O1 Ta1 Cl3 89.94(5) . . ?
O1 Ta1 Cl3 90.06(5) . 3_666 ?
O1 Ta1 Cl3 89.94(5) 3_666 3_666 ?
O1 Ta1 Cl1 89.95(5) 3_666 3_666 ?
O1 Ta1 Cl1 90.05(5) 3_666 . ?
O1 Ta1 Cl1 90.05(5) . 3_666 ?
O1 Ta1 Cl1 89.95(5) . . ?
O1 Ta1 O1 180.0 3_666 . ?
C1 O1 Ta1 123.61(13) . . ?
C1 O1 C2 114.07(18) . . ?
C2 O1 Ta1 122.32(14) . . ?
O1 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
O1 C1 C3 112.5(2) . . ?
H1A C1 H1B 107.8 . . ?
C3 C1 H1A 109.1 . . ?
C3 C1 H1B 109.1 . . ?
O1 C2 H2A 109.1 . . ?
O1 C2 H2B 109.1 . . ?
O1 C2 C4 112.45(19) . . ?
H2A C2 H2B 107.8 . . ?
C4 C2 H2A 109.1 . . ?
C4 C2 H2B 109.1 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

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
Ta1 O1 C1 C3 114.91(19) . . . . ?
Ta1 O1 C2 C4 117.30(19) . . . . ?
C1 O1 C2 C4 -62.4(3) . . . . ?
C2 O1 C1 C3 -65.4(3) . . . . ?


_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 1.659
_oxdiff_exptl_absorpt_empirical_full_min 0.822
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_363
_database_code_depnum_ccdc_archive 'CCDC 2254036'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2023-04-05 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_audit_creation_date             2022-10-13
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'Tetrachloro-bis(diethyl ether)niobium(IV)'
_chemical_formula_moiety         'C4 H10 Cl2 Nb0.5 O'
_chemical_formula_sum            'C4 H10 Cl2 Nb0.50 O'
_chemical_formula_weight         191.47
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Nb Cl O C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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                   7.6027(2)
_cell_length_b                   11.3827(3)
_cell_length_c                   8.9641(3)
_cell_angle_alpha                90
_cell_angle_beta                 107.012(3)
_cell_angle_gamma                90
_cell_volume                     741.80(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4053
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6040
_cell_measurement_theta_min      2.9630
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.513
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.937
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
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_absorpt_special_details   ?
_exptl_crystal_colour            'dull dark yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             386
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -2 -1 0.0657
-5 14 -1 0.0685
0 -8 10 0.0642
7 -3 -11 0.0838
1 -2 12 0.0766
7 -5 5 0.0857
9 -4 -9 0.0905
-9 6 -3 0.0691
0 2 -12 0.0724
-4 4 -9 0.0618
-9 4 9 0.1169
9 1 4 0.0937
9 0 -9 0.0973
-5 -1 -9 0.0595
-10 -1 0 0.0843
-9 -1 -3 0.0722
-8 -9 -2 0.0688
-4 -7 -9 0.0551
-9 -6 8 0.1035
9 9 0 0.0872
0 4 12 0.0822
7 4 -11 0.0877
-2 -16 3 0.0574
1 -14 -6 0.0572
1 16 -2 0.0533
-3 -12 9 0.0706
-2 12 8 0.0706
-3 -15 0 0.0498
2 -7 -11 0.0696

_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.112
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
1.0012 -2.0011 -1.0016 -0.0086 0.1398 0.0873
-5.2719 13.5406 -0.7484 -0.0000 -1.0000 -0.0000
0.3285 -8.2345 10.2567 0.0000 0.6306 -0.7761
7.0237 -2.5567 -11.3535 0.2183 0.3005 0.9285
0.6893 -2.2903 11.7006 0.2629 0.3618 -0.8944
7.4893 -5.4518 5.0203 0.5554 0.7645 -0.3271
8.9749 -4.1560 -8.9217 0.3842 0.5288 0.7568
-8.6550 5.7977 -2.6432 -0.5824 -0.8016 0.1351
-0.4967 2.1849 -11.7905 -0.2527 -0.3478 0.9029
-4.4707 4.2056 -8.9737 -0.4442 -0.6114 0.6549
-9.0477 4.2249 8.7727 -0.3915 -0.5388 -0.7459
8.6110 0.7500 4.2005 0.8348 0.4820 -0.2659
9.3657 0.1279 -9.1222 0.5544 0.3201 0.7682
-4.6995 -0.7575 -9.2233 -0.6346 -0.3664 0.6805
-10.2554 -0.6391 0.0542 -0.8637 -0.4986 -0.0739
-9.4143 -0.7150 -2.5028 -0.8588 -0.4958 0.1293
-8.1160 -8.5914 -1.7226 -0.9959 0.0000 0.0905
-3.6279 -6.5786 -8.9802 -0.7348 0.0000 0.6783
-8.8080 -5.9317 8.3019 -0.7220 0.0000 -0.6919
8.6327 8.5717 0.1332 0.9994 -0.0000 0.0357
0.0326 3.9357 11.7041 0.4167 -0.0000 -0.9091
7.3464 3.6160 -10.9163 0.4614 -0.0000 0.8872
-1.5513 -15.5382 2.9911 -0.5738 0.7898 -0.2169
1.2551 -14.1410 -5.9522 -0.5123 0.7051 0.4903
1.1773 15.8489 -1.7337 0.5838 -0.8035 0.1168
-3.1023 -11.7414 8.5381 -0.4407 0.6066 -0.6616
-2.0056 12.2599 8.1446 0.4407 -0.6066 -0.6616
-2.7894 -15.4449 0.0671 -0.7431 0.6691 0.0000
2.2051 -7.2576 -11.2464 -0.3323 0.2992 0.8944

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6073
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.478
_diffrn_reflns_theta_min         2.975
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -2.00  76.50   0.50   13.50    --   20.00  54.00 -90.00  157
  2  ω    -33.00   0.00   0.50   13.50    --   20.00  54.00  60.00   66
  3  ω     -5.00  21.00   0.50   13.50    --   20.00  54.00-180.00   52
  4  ω     68.00  94.00   0.50   13.50    --   20.00  54.00-180.00   52
  5  ω    -74.00  65.00   0.50   13.50    --   20.00  54.00  30.00  278
  6  ω    -69.00 -27.00   0.50   13.50    --   20.00  54.00 -30.00   84
  7  ω    -20.00 101.00   0.50   13.50    --   20.00  54.00 -30.00  242
  8  ω    -67.00 -40.00   0.50   13.50    --   20.00  54.00  90.00   54
  9  ω     64.00  89.00   0.50   13.50    --   20.00  54.00  90.00   50
 10  ω    -68.00 -42.00   0.50   13.50    --   20.00  54.00 -90.00   52
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0822638000
_diffrn_orient_matrix_UB_12      0.0333636000
_diffrn_orient_matrix_UB_13      0.0241506000
_diffrn_orient_matrix_UB_21      0.0519951000
_diffrn_orient_matrix_UB_22      -0.0526380000
_diffrn_orient_matrix_UB_23      0.0175555000
_diffrn_orient_matrix_UB_31      0.0068939000
_diffrn_orient_matrix_UB_32      -0.0015803000
_diffrn_orient_matrix_UB_33      -0.0771584000
_diffrn_oxdiff_digest_frames     
;
016a43076073660edbe4f027252c6c3e6201087d8e3
;
_diffrn_oxdiff_digest_hkl        
;
0163f7340304b3f92d28658dac6bdcf1514f11
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1467
_reflns_number_total             1677
_reflns_odcompleteness_completeness 98.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (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         0.862
_refine_diff_density_min         -0.895
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1677
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0255
_refine_ls_restrained_S_all      1.052
_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)+(0.0411P)²+0.0069P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0668
_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.a Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), 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
Nb1 Nb 0.500000 0.500000 0.500000 0.01230(10) Uani 1 2 d S T P . .
Cl2 Cl 0.49501(7) 0.63056(5) 0.29073(6) 0.01985(14) Uani 1 1 d . . . . .
Cl3 Cl 0.81713(7) 0.54081(5) 0.62423(6) 0.02053(14) Uani 1 1 d . . . . .
O4 O 0.42405(18) 0.64052(12) 0.62426(17) 0.0156(3) Uani 1 1 d . . . . .
C5 C 0.2755(3) 0.6297(2) 0.6987(3) 0.0190(5) Uani 1 1 d . . . . .
H5A H 0.217686 0.553314 0.673972 0.023 Uiso 1 1 calc R . . . .
H5B H 0.182971 0.689092 0.656243 0.023 Uiso 1 1 calc R . . . .
C7 C 0.5149(3) 0.75639(18) 0.6446(3) 0.0194(5) Uani 1 1 d . . . . .
H7A H 0.619587 0.753355 0.603574 0.023 Uiso 1 1 calc R . . . .
H7B H 0.560496 0.774229 0.755051 0.023 Uiso 1 1 calc R . . . .
C6 C 0.3449(3) 0.6435(2) 0.8735(3) 0.0257(5) Uani 1 1 d . . . . .
H6A H 0.380076 0.723695 0.898885 0.039 Uiso 1 1 calc GR . . . .
H6B H 0.449420 0.593293 0.914429 0.039 Uiso 1 1 calc GR . . . .
H6C H 0.249299 0.622185 0.918591 0.039 Uiso 1 1 calc GR . . . .
C8 C 0.3874(3) 0.8527(2) 0.5636(3) 0.0256(5) Uani 1 1 d . . . . .
H8A H 0.337656 0.833799 0.455004 0.038 Uiso 1 1 calc GR . . . .
H8B H 0.454065 0.925360 0.574185 0.038 Uiso 1 1 calc GR . . . .
H8C H 0.288945 0.860535 0.609862 0.038 Uiso 1 1 calc GR . . . .


_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
Nb1 Cl2 2.3848(5) . ?
Nb1 Cl2 2.3848(5) 3_666 ?
Nb1 Cl3 2.3870(5) 3_666 ?
Nb1 Cl3 2.3870(5) . ?
Nb1 O4 2.1235(14) . ?
Nb1 O4 2.1235(14) 3_666 ?
O4 C5 1.475(2) . ?
O4 C7 1.475(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.509(3) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C7 C8 1.503(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?

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
Cl2 Nb1 Cl2 180.0 . 3_666 ?
Cl2 Nb1 Cl3 88.444(19) 3_666 . ?
Cl2 Nb1 Cl3 88.444(19) . 3_666 ?
Cl2 Nb1 Cl3 91.556(19) 3_666 3_666 ?
Cl2 Nb1 Cl3 91.556(19) . . ?
Cl3 Nb1 Cl3 180.0 . 3_666 ?
O4 Nb1 Cl2 90.05(4) 3_666 . ?
O4 Nb1 Cl2 90.06(4) . 3_666 ?
O4 Nb1 Cl2 89.95(4) . . ?
O4 Nb1 Cl2 89.95(4) 3_666 3_666 ?
O4 Nb1 Cl3 89.93(4) 3_666 . ?
O4 Nb1 Cl3 89.93(4) . 3_666 ?
O4 Nb1 Cl3 90.07(4) . . ?
O4 Nb1 Cl3 90.07(4) 3_666 3_666 ?
O4 Nb1 O4 180.0 3_666 . ?
C5 O4 Nb1 122.39(12) . . ?
C5 O4 C7 114.32(15) . . ?
C7 O4 Nb1 123.29(11) . . ?
O4 C5 H5A 109.1 . . ?
O4 C5 H5B 109.1 . . ?
O4 C5 C6 112.34(17) . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 H5A 109.1 . . ?
C6 C5 H5B 109.1 . . ?
O4 C7 H7A 109.1 . . ?
O4 C7 H7B 109.1 . . ?
O4 C7 C8 112.34(17) . . ?
H7A C7 H7B 107.9 . . ?
C8 C7 H7A 109.1 . . ?
C8 C7 H7B 109.1 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?

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
Nb1 O4 C5 C6 116.94(18) . . . . ?
Nb1 O4 C7 C8 114.75(17) . . . . ?
C5 O4 C7 C8 -65.6(2) . . . . ?
C7 O4 C5 C6 -62.7(2) . . . . ?

_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 1.237
_oxdiff_exptl_absorpt_empirical_full_min 0.825
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_348
_database_code_depnum_ccdc_archive 'CCDC 2254039'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2023-04-05 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_audit_creation_date             2023-04-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        
'Hexachloro-bis(1,2-dimethoxyethane)ditantalum(III,IV) hexachlorotantalate(V)'
_chemical_formula_moiety         'C8 H20 Cl6 O4 Ta2, Cl6 Ta'
_chemical_formula_sum            'C8 H20 Cl12 O4 Ta3'
_chemical_formula_weight         1148.49
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta3 Cl12 O4 C8 H20'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.0261(6)
_cell_length_b                   7.2740(5)
_cell_length_c                   13.2064(5)
_cell_angle_alpha                85.923(5)
_cell_angle_beta                 85.482(6)
_cell_angle_gamma                81.744(7)
_cell_volume                     664.66(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4039
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6350
_cell_measurement_theta_min      1.5580
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    13.536
_exptl_absorpt_correction_T_max  0.422
_exptl_absorpt_correction_T_min  0.144
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
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)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    2.869
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             523
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 -1 0 0.0861
-3 -6 -15 0.0197
3 6 15 0.0552
0 7 -12 0.0641
9 4 0 0.0415
1 -7 12 0.0753

_exptl_crystal_size_max          0.234
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.076
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
-2.0015 -1.0005 0.0018 0.0388 -0.0228 -0.2098
-2.8554 -6.4410 -15.0218 -0.0992 -0.9435 -0.3162
2.5659 6.2991 15.3020 0.1003 0.9541 0.2822
-0.0466 7.2535 -12.1470 0.7986 -0.3556 0.4856
9.4115 4.3986 -0.1228 -0.2054 0.0915 0.9744
0.8347 -7.0300 12.3785 -0.8317 0.3703 -0.4138

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0903
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6551
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         2.835
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     20.00  46.00   0.50   15.00    --   20.00  54.00 -60.00   52
  2  ω    -74.00  71.00   0.50   15.00    --   20.00  54.00-180.00  290
  3  ω    -58.00 -32.00   0.50   15.00    --   20.00  54.00 120.00   52
  4  ω     52.00  78.00   0.50   15.00    --   20.00  54.00 120.00   52
  5  ω    -73.00 103.00   0.50   15.00    --   20.00  54.00-120.00  352
  6  ω    -74.00  31.00   0.50   15.00    --   20.00  54.00 -30.00  210
  7  ω     82.00 107.00   0.50   15.00    --   20.00  54.00 -30.00   50
  8  ω    -74.00 -27.00   0.50   15.00    --   20.00  54.00  90.00   94
  9  ω     25.00  51.00   0.50   15.00    --   20.00  54.00  90.00   52
 10  ω    -64.00  -5.00   0.50   15.00    --   20.00  54.00   0.00  118
 11  ω     75.00 100.00   0.50   15.00    --   20.00  54.00   0.00   50
 12  ω    -55.00 -30.00   0.50   15.00    --   20.00  54.00 150.00   50
 13  ω     80.00 105.00   0.50   15.00    --   20.00  54.00 150.00   50
 14  ω    -27.00  -2.00   0.50   15.00    --   20.00  54.00 -60.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0601036000
_diffrn_orient_matrix_UB_12      0.0814282000
_diffrn_orient_matrix_UB_13      -0.0168883000
_diffrn_orient_matrix_UB_21      -0.0053718000
_diffrn_orient_matrix_UB_22      0.0336650000
_diffrn_orient_matrix_UB_23      0.0493943000
_diffrn_orient_matrix_UB_31      0.0825539000
_diffrn_orient_matrix_UB_32      0.0445024000
_diffrn_orient_matrix_UB_33      -0.0137225000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2159
_reflns_number_total             2864
_reflns_odcompleteness_completeness 97.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 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  (Sheldrick, 2015)'
_refine_diff_density_max         3.003
_refine_diff_density_min         -2.561
_refine_diff_density_rms         0.367
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2864
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0460
_refine_ls_restrained_S_all      0.956
_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)+(0.0444P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0935
_refine_ls_wR_factor_ref         0.0990
_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.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_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
Ta1 Ta 0.09067(5) 0.52615(5) 0.08733(3) 0.01530(13) Uani 1 1 d . . . . .
Ta2 Ta 0.500000 1.000000 0.500000 0.01858(16) Uani 1 2 d S . P . .
Cl3 Cl -0.1270(3) 0.3007(3) 0.07470(17) 0.0191(5) Uani 1 1 d . . . . .
Cl4 Cl 0.3678(3) 0.3122(3) 0.05504(18) 0.0198(5) Uani 1 1 d . . . . .
Cl5 Cl -0.1514(3) 0.7532(3) 0.15576(19) 0.0255(6) Uani 1 1 d . . . . .
Cl6 Cl 0.4784(4) 0.8779(4) 0.66956(18) 0.0290(6) Uani 1 1 d . . . . .
Cl7 Cl 0.6941(4) 0.7238(4) 0.4510(2) 0.0347(7) Uani 1 1 d . . . . .
Cl8 Cl 0.2247(4) 0.8736(4) 0.4672(2) 0.0336(6) Uani 1 1 d . . . . .
O9 O 0.1135(9) 0.4208(9) 0.2457(5) 0.0221(15) Uani 1 1 d . . . . .
O12 O 0.2889(9) 0.6946(9) 0.1400(5) 0.0215(16) Uani 1 1 d . . . . .
C13 C 0.2911(14) 0.8912(12) 0.1259(7) 0.022(2) Uani 1 1 d . . . . .
H13A H 0.246615 0.934795 0.060375 0.032 Uiso 1 1 calc R U . . .
H13B H 0.420114 0.917894 0.129757 0.032 Uiso 1 1 calc R U . . .
H13C H 0.207954 0.952798 0.178033 0.032 Uiso 1 1 calc R U . . .
C14 C -0.0200(13) 0.3201(13) 0.3112(7) 0.024(2) Uani 1 1 d . . . . .
H14A H -0.125095 0.406878 0.337550 0.036 Uiso 1 1 calc R U . . .
H14B H 0.046552 0.254614 0.366640 0.036 Uiso 1 1 calc R U . . .
H14C H -0.069002 0.232773 0.272404 0.036 Uiso 1 1 calc R U . . .
C10 C 0.2021(14) 0.5443(14) 0.3024(7) 0.024(2) Uani 1 1 d . . . . .
H10A H 0.249873 0.479138 0.363974 0.029 Uiso 1 1 calc R U . . .
H10B H 0.108017 0.649372 0.321621 0.029 Uiso 1 1 calc R U . . .
C11 C 0.3672(14) 0.6119(14) 0.2360(7) 0.025(2) Uani 1 1 d . . . . .
H11A H 0.421681 0.704146 0.269989 0.029 Uiso 1 1 calc R U . . .
H11B H 0.467763 0.508852 0.222489 0.029 Uiso 1 1 calc R U . . .


_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
Ta1 Ta1 2.7956(7) 2_565 ?
Ta1 Cl3 2.420(2) . ?
Ta1 Cl3 2.419(2) 2_565 ?
Ta1 Cl4 2.343(2) . ?
Ta1 Cl5 2.366(2) . ?
Ta1 O9 2.186(6) . ?
Ta1 O12 2.165(6) . ?
Ta2 Cl6 2.351(2) 2_676 ?
Ta2 Cl6 2.351(2) . ?
Ta2 Cl7 2.361(2) 2_676 ?
Ta2 Cl7 2.361(2) . ?
Ta2 Cl8 2.340(3) . ?
Ta2 Cl8 2.340(3) 2_676 ?
O9 C14 1.465(10) . ?
O9 C10 1.444(11) . ?
O12 C13 1.431(10) . ?
O12 C11 1.476(10) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.516(13) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?

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
Cl3 Ta1 Ta1 54.72(6) 2_565 2_565 ?
Cl3 Ta1 Ta1 54.70(5) . 2_565 ?
Cl3 Ta1 Cl3 109.42(6) 2_565 . ?
Cl4 Ta1 Ta1 96.76(6) . 2_565 ?
Cl4 Ta1 Cl3 93.81(8) . . ?
Cl4 Ta1 Cl3 93.99(8) . 2_565 ?
Cl4 Ta1 Cl5 166.01(8) . . ?
Cl5 Ta1 Ta1 97.23(6) . 2_565 ?
Cl5 Ta1 Cl3 94.33(8) . . ?
Cl5 Ta1 Cl3 94.01(8) . 2_565 ?
O9 Ta1 Ta1 141.41(18) . 2_565 ?
O9 Ta1 Cl3 163.87(19) . 2_565 ?
O9 Ta1 Cl3 86.71(18) . . ?
O9 Ta1 Cl4 84.72(17) . . ?
O9 Ta1 Cl5 84.41(17) . . ?
O12 Ta1 Ta1 140.75(17) . 2_565 ?
O12 Ta1 Cl3 164.54(17) . . ?
O12 Ta1 Cl3 86.04(17) . 2_565 ?
O12 Ta1 Cl4 84.51(17) . . ?
O12 Ta1 Cl5 84.61(18) . . ?
O12 Ta1 O9 77.8(2) . . ?
Cl6 Ta2 Cl6 180.0 . 2_676 ?
Cl6 Ta2 Cl7 90.32(9) . . ?
Cl6 Ta2 Cl7 89.68(9) 2_676 . ?
Cl6 Ta2 Cl7 90.33(9) 2_676 2_676 ?
Cl6 Ta2 Cl7 89.68(9) . 2_676 ?
Cl7 Ta2 Cl7 180.00(15) . 2_676 ?
Cl8 Ta2 Cl6 90.50(10) . . ?
Cl8 Ta2 Cl6 89.50(10) 2_676 . ?
Cl8 Ta2 Cl6 89.50(10) . 2_676 ?
Cl8 Ta2 Cl6 90.50(10) 2_676 2_676 ?
Cl8 Ta2 Cl7 90.25(10) . 2_676 ?
Cl8 Ta2 Cl7 90.25(10) 2_676 . ?
Cl8 Ta2 Cl7 89.75(10) . . ?
Cl8 Ta2 Cl7 89.75(10) 2_676 2_676 ?
Cl8 Ta2 Cl8 180.0 . 2_676 ?
Ta1 Cl3 Ta1 70.58(6) 2_565 . ?
C14 O9 Ta1 128.8(5) . . ?
C10 O9 Ta1 111.1(5) . . ?
C10 O9 C14 111.6(7) . . ?
C13 O12 Ta1 129.4(5) . . ?
C13 O12 C11 113.6(7) . . ?
C11 O12 Ta1 110.9(5) . . ?
O12 C13 H13A 109.5 . . ?
O12 C13 H13B 109.5 . . ?
O12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O9 C14 H14A 109.5 . . ?
O9 C14 H14B 109.5 . . ?
O9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O9 C10 H10A 110.0 . . ?
O9 C10 H10B 110.0 . . ?
O9 C10 C11 108.5(7) . . ?
H10A C10 H10B 108.4 . . ?
C11 C10 H10A 110.0 . . ?
C11 C10 H10B 110.0 . . ?
O12 C11 C10 107.5(7) . . ?
O12 C11 H11A 110.2 . . ?
O12 C11 H11B 110.2 . . ?
C10 C11 H11A 110.2 . . ?
C10 C11 H11B 110.2 . . ?
H11A C11 H11B 108.5 . . ?

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
Ta1 O9 C10 C11 -40.8(8) . . . . ?
Ta1 O12 C11 C10 -41.9(8) . . . . ?
O9 C10 C11 O12 54.6(10) . . . . ?
C13 O12 C11 C10 113.3(9) . . . . ?
C14 O9 C10 C11 168.2(7) . . . . ?


_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 7.236
_oxdiff_exptl_absorpt_empirical_full_min 0.599
_oxdiff_exptl_absorpt_spherical_max 0.274
_oxdiff_exptl_absorpt_spherical_min 0.252
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: 1,2-dimethoxyethane'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_286
_database_code_depnum_ccdc_archive 'CCDC 2254038'
loop_
_audit_author_name
_audit_author_address
'Thomas Shaw'
;University of Central Florida
United States of America
;
_audit_update_record             
;
2023-04-05 deposited with the CCDC.	2023-06-19 downloaded from the CCDC.
;
_audit_creation_date             2022-11-02
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        'bis(diethyl ether)ocatchloro ditantalum(IV)'
_chemical_formula_moiety         'C8 H20 Cl8 O2 Ta2'
_chemical_formula_sum            'C8 H20 Cl8 O2 Ta2'
_chemical_formula_weight         793.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ta Cl O C H'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ta Ta -0.7052 6.5227 '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                   7.8857(2)
_cell_length_b                   11.5388(4)
_cell_length_c                   11.4054(4)
_cell_angle_alpha                90
_cell_angle_beta                 103.223(3)
_cell_angle_gamma                90
_cell_volume                     1010.28(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4244
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.6390
_cell_measurement_theta_min      2.5410
_shelx_estimated_absorpt_T_max   0.450
_shelx_estimated_absorpt_T_min   0.130
_exptl_absorpt_coefficient_mu    11.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.21674
_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 yellowish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.609
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             732
_exptl_crystal_preparation       
'A pipet of room temperature diethyl ether was slowly added to a small amount of solid tantalum(IV) chloride, which was obtained via the solution state reduction of tantalum(V) chloride with dimethylphenylsilane. This addition of ether resulted in a blue-green solution.'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.614
_diffrn_reflns_theta_min         2.860
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     57.00  83.00   0.50   15.06    --   20.00  54.00  60.00   52
  2  ω    -68.00  65.00   0.50   15.06    --   20.00  54.00-120.00  266
  3  ω     70.00 107.00   0.50   15.06    --   20.00  54.00-120.00   74
  4  ω    -74.00 107.00   0.50   15.06    --   20.00  54.00 150.00  362
  5  ω    -74.00 -49.00   0.50   15.06    --   20.00  54.00 -60.00   50
  6  ω    -27.00  -2.00   0.50   15.06    --   20.00  54.00 -60.00   50
  7  ω      0.00  25.00   0.50   15.06    --   20.00  54.00 -60.00   50
  8  ω     33.00  58.00   0.50   15.06    --   20.00  54.00 -60.00   50
  9  ω    -53.00 -18.00   0.50   15.06    --   20.00  54.00   0.00   70
 10  ω     40.00  65.00   0.50   15.06    --   20.00  54.00   0.00   50
 11  ω    -11.00  14.00   0.50   15.06    --   20.00  54.00  60.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0431456000
_diffrn_orient_matrix_UB_12      0.0237048000
_diffrn_orient_matrix_UB_13      -0.0425732000
_diffrn_orient_matrix_UB_21      -0.0657677000
_diffrn_orient_matrix_UB_22      -0.0226856000
_diffrn_orient_matrix_UB_23      -0.0475236000
_diffrn_orient_matrix_UB_31      -0.0483979000
_diffrn_orient_matrix_UB_32      0.0521018000
_diffrn_orient_matrix_UB_33      -0.0012995000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2362
_reflns_number_total             2996
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         2.050
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2996
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0341
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0312P)²+1.6982P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0767
_refine_special_details          ?
_olex2_refinement_description    
;
1. Uiso/Uaniso restraints and constraints
Uanis(Cl6) \\sim Ueq, Uanis(Cl5) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
2. Others
 Sof(Ta2)=Sof(Cl5)=Sof(Cl6)=Sof(Cl7)=1-FVAR(1)
 Sof(Ta1)=Sof(Cl2)=Sof(Cl4)=Sof(Cl1)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C5(H5A,H5B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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
Ta1 Ta 0.50226(5) 0.45568(4) 0.62736(3) 0.01449(11) Uani 0.942(2) 1 d . . P A 1
Cl2 Cl 0.20376(17) 0.48374(14) 0.59963(14) 0.0216(3) Uani 0.942(2) 1 d . . P A
1
Cl3 Cl 0.55840(18) 0.65005(12) 0.56788(13) 0.0226(3) Uani 1 1 d . . . . .
Cl4 Cl 0.78704(18) 0.38923(14) 0.66252(14) 0.0212(3) Uani 0.942(2) 1 d . . P A
1
Cl1 Cl 0.5571(2) 0.53927(16) 0.82297(17) 0.0227(3) Uani 0.942(2) 1 d . . P A 1
O1 O 0.4470(5) 0.2896(3) 0.7036(3) 0.0206(9) Uani 1 1 d . . . . .
C2 C 0.3302(10) 0.2013(7) 0.6413(7) 0.0426(19) Uani 1 1 d . . . . .
H2A H 0.253357 0.235643 0.571295 0.051 Uiso 1 1 calc R U . . .
H2B H 0.258607 0.173428 0.694192 0.051 Uiso 1 1 calc R U . . .
C3 C 0.3777(11) 0.2878(7) 0.9025(7) 0.047(2) Uani 1 1 d . . . . .
H3A H 0.269711 0.250734 0.865544 0.071 Uiso 1 1 calc R U . . .
H3B H 0.360496 0.370167 0.903544 0.071 Uiso 1 1 calc R U . . .
H3C H 0.417059 0.260121 0.983540 0.071 Uiso 1 1 calc R U . . .
C4 C 0.4223(11) 0.1012(6) 0.6019(7) 0.045(2) Uani 1 1 d . . . . .
H4A H 0.502581 0.128867 0.556458 0.068 Uiso 1 1 calc R U . . .
H4B H 0.338870 0.050605 0.552517 0.068 Uiso 1 1 calc R U . . .
H4C H 0.484832 0.059612 0.671298 0.068 Uiso 1 1 calc R U . . .
C5 C 0.5067(10) 0.2615(7) 0.8346(7) 0.046(2) Uani 1 1 d . . . . .
H5A H 0.535271 0.179700 0.843258 0.056 Uiso 1 1 calc R U . . .
H5B H 0.612019 0.304953 0.867967 0.056 Uiso 1 1 calc R U . . .
Ta2 Ta 0.5562(14) 0.4132(9) 0.6017(8) 0.038(3) Uani 0.058(2) 1 d . . P A 2
Cl5 Cl 0.264(4) 0.466(2) 0.521(3) 0.031(6) Uani 0.058(2) 1 d . U P A 2
Cl6 Cl 0.837(4) 0.347(3) 0.705(3) 0.030(6) Uani 0.058(2) 1 d . U P A 2
Cl7 Cl 0.551(5) 0.529(3) 0.763(4) 0.049(12) Uani 0.058(2) 1 d . . 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
Ta1 Ta1 3.0725(6) 3_666 ?
Ta1 Cl2 2.3249(14) . ?
Ta1 Cl3 2.4132(15) . ?
Ta1 Cl3 2.4876(15) 3_666 ?
Ta1 Cl4 2.3195(15) . ?
Ta1 Cl1 2.3776(19) . ?
Ta1 O1 2.189(4) . ?
Cl3 Ta2 2.761(9) . ?
Cl3 Ta2 2.072(9) 3_666 ?
Cl3 Cl5 2.34(3) 3_666 ?
O1 C2 1.447(7) . ?
O1 C5 1.496(8) . ?
O1 Ta2 2.141(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C4 1.488(10) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3 C5 1.445(10) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
Ta2 Ta2 3.040(12) 3_666 ?
Ta2 Cl5 2.61(3) 3_666 ?
Ta2 Cl5 2.36(3) . ?
Ta2 Cl6 2.38(3) . ?
Ta2 Cl7 2.28(4) . ?

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
Cl2 Ta1 Ta1 91.87(4) . 3_666 ?
Cl2 Ta1 Cl3 94.44(5) . . ?
Cl2 Ta1 Cl3 88.00(5) . 3_666 ?
Cl2 Ta1 Cl1 91.85(6) . . ?
Cl3 Ta1 Ta1 50.10(4) 3_666 3_666 ?
Cl3 Ta1 Ta1 52.26(4) . 3_666 ?
Cl3 Ta1 Cl3 102.37(4) . 3_666 ?
Cl4 Ta1 Ta1 94.29(5) . 3_666 ?
Cl4 Ta1 Cl2 168.43(6) . . ?
Cl4 Ta1 Cl3 97.08(5) . . ?
Cl4 Ta1 Cl3 88.45(5) . 3_666 ?
Cl4 Ta1 Cl1 90.62(6) . . ?
Cl1 Ta1 Ta1 135.43(5) . 3_666 ?
Cl1 Ta1 Cl3 83.17(6) . . ?
Cl1 Ta1 Cl3 174.46(6) . 3_666 ?
O1 Ta1 Ta1 134.97(11) . 3_666 ?
O1 Ta1 Cl2 83.61(10) . . ?
O1 Ta1 Cl3 84.92(11) . 3_666 ?
O1 Ta1 Cl3 172.42(11) . . ?
O1 Ta1 Cl4 85.11(11) . . ?
O1 Ta1 Cl1 89.56(11) . . ?
Ta1 Cl3 Ta1 77.63(4) . 3_666 ?
Ta2 Cl3 Ta2 76.5(2) 3_666 . ?
Ta2 Cl3 Cl5 64.4(8) 3_666 3_666 ?
Cl5 Cl3 Ta2 61.0(8) 3_666 . ?
C2 O1 Ta1 125.7(4) . . ?
C2 O1 C5 110.9(5) . . ?
C2 O1 Ta2 119.5(4) . . ?
C5 O1 Ta1 122.7(4) . . ?
C5 O1 Ta2 127.8(4) . . ?
O1 C2 H2A 108.9 . . ?
O1 C2 H2B 108.9 . . ?
O1 C2 C4 113.3(6) . . ?
H2A C2 H2B 107.7 . . ?
C4 C2 H2A 108.9 . . ?
C4 C2 H2B 108.9 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C3 H3A 109.5 . . ?
C5 C3 H3B 109.5 . . ?
C5 C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C5 H5A 109.0 . . ?
O1 C5 H5B 109.0 . . ?
C3 C5 O1 113.0(6) . . ?
C3 C5 H5A 109.0 . . ?
C3 C5 H5B 109.0 . . ?
H5A C5 H5B 107.8 . . ?
Cl3 Ta2 Cl3 103.5(2) 3_666 . ?
Cl3 Ta2 O1 97.4(3) 3_666 . ?
Cl3 Ta2 Ta2 41.5(3) . 3_666 ?
Cl3 Ta2 Ta2 62.0(3) 3_666 3_666 ?
Cl3 Ta2 Cl5 82.0(7) 3_666 3_666 ?
Cl3 Ta2 Cl5 63.3(8) 3_666 . ?
Cl3 Ta2 Cl6 120.4(10) 3_666 . ?
Cl3 Ta2 Cl7 151.1(10) 3_666 . ?
O1 Ta2 Cl3 138.7(8) . . ?
O1 Ta2 Ta2 140.4(6) . 3_666 ?
O1 Ta2 Cl5 168.8(10) . 3_666 ?
O1 Ta2 Cl5 84.6(8) . . ?
O1 Ta2 Cl6 87.8(8) . . ?
O1 Ta2 Cl7 82.5(13) . . ?
Cl5 Ta2 Cl3 51.5(6) 3_666 . ?
Cl5 Ta2 Cl3 74.0(7) . . ?
Cl5 Ta2 Cl5 104.9(9) . 3_666 ?
Cl5 Ta2 Cl6 171.9(12) . . ?
Cl6 Ta2 Cl3 110.6(8) . . ?
Cl6 Ta2 Cl5 83.0(11) . 3_666 ?
Cl7 Ta2 Cl3 62.3(13) . . ?
Cl7 Ta2 Cl5 103.5(15) . 3_666 ?
Cl7 Ta2 Cl5 88.1(12) . . ?
Cl7 Ta2 Cl6 88.5(10) . . ?
Cl3 Cl5 Ta2 67.5(9) 3_666 3_666 ?
Cl3 Cl5 Ta2 52.3(7) 3_666 . ?

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
Ta1 O1 C2 C4 103.4(6) . . . . ?
Ta1 O1 C5 C3 93.4(6) . . . . ?
C2 O1 C5 C3 -78.2(8) . . . . ?
C5 O1 C2 C4 -85.2(7) . . . . ?
Ta2 O1 C2 C4 80.9(8) . . . . ?
Ta2 O1 C5 C3 117.1(8) . . . . ?


_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 3.377
_oxdiff_exptl_absorpt_empirical_full_min 0.708
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl ether'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
