#------------------------------------------------------------------------------
#$Date: 2019-11-10 06:47:08 +0100 (dom 10 de nov de 2019) $
#$Revision: 225905 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/57/4515780.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4515780
loop_
_publ_author_name
'Messinis, Antonis M.'
'Wright, William R. H.'
'Batsanov, Andrei S.'
'Howard, Judith A. K.'
'Hanton, Martin J.'
'Dyer, Philip W.'
_publ_section_title
;
 Exploration of Homogeneous Ethylene Dimerization Mediated by Tungsten
 Mono(imido) Complexes
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11235
_journal_paper_doi               10.1021/acscatal.8b02201
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C4 H10 Cl8 N2 W2'
_chemical_formula_sum            'C4 H10 Cl8 N2 W2'
_chemical_formula_weight         737.44
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-07-28
_audit_creation_method
;
  Olex2 1.2-alpha
  (compiled 2012.07.25 svn.r2431, GUI svn.r4294)
;
_cell_angle_alpha                97.754(3)
_cell_angle_beta                 108.946(3)
_cell_angle_gamma                112.350(4)
_cell_formula_units_Z            1
_cell_length_a                   7.7134(3)
_cell_length_b                   7.8170(3)
_cell_length_c                   7.9908(3)
_cell_measurement_reflns_used    4387
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.2798
_cell_measurement_theta_min      2.8153
_cell_volume                     402.67(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device
'Agilent Technologies, Gemini S Ultra kappa-diffractometer'
_diffrn_measurement_device_type  'Sapphire3 CCD area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0389031000
_diffrn_orient_matrix_UB_12      -0.0418026000
_diffrn_orient_matrix_UB_13      0.0615255000
_diffrn_orient_matrix_UB_21      0.0129479000
_diffrn_orient_matrix_UB_22      0.0910885000
_diffrn_orient_matrix_UB_23      0.0458867000
_diffrn_orient_matrix_UB_31      -0.1010207000
_diffrn_orient_matrix_UB_32      -0.0223753000
_diffrn_orient_matrix_UB_33      -0.0613066000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0470
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10156
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         32.35
_diffrn_reflns_theta_min         2.82
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    15.575
_exptl_absorpt_correction_T_max  0.4345
_exptl_absorpt_correction_T_min  0.3540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS 2009/1, R(int)=0.1296 before correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    3.041
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.359
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.253
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         2654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0270P)²+0.1107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0642
_refine_ls_wR_factor_ref         0.0665
_reflns_number_gt                2463
_reflns_number_total             2654
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           1a
_cod_database_code               4515780
_ccdc_comments                   'redetermination of SEPHAW'
_shelx_res_file
;
TITL 12SRV133 in P-1 #2
CELL 0.71073 7.71338 7.817013 7.990791 97.7544 108.9457 112.35
ZERR 1 0.000298 0.000297 0.000281 0.003 0.0034 0.0036
LATT 1
 
SFAC C H N Cl W
UNIT 4 10 2 8 2
 
L.S. 7 0 0 511
PLAN  7
TEMP -153.15
REM reset to P-1 #2
BOND $H
REM OMIT -3 60
fmap 2
acta 60
OMIT 1 0 0
OMIT 0 -4 5
OMIT -2 4 2
OMIT -6 4 2
OMIT -4 4 4
OMIT -4 4 2
REM <HKL>I:/andrei/datasets/12srv133/12SRV133.hkl</HKL>
 
WGHT    0.027000    0.110700
FVAR       0.46034
W     5    0.238503    0.404996    0.273913    11.00000    0.01614    0.01513 =
         0.01780    0.00775    0.00810    0.00748
CL1   4    0.345480    0.415826    0.599473    11.00000    0.01837    0.01780 =
         0.01815    0.00918    0.00960    0.00782
CL2   4    0.284599    0.716938    0.369659    11.00000    0.02234    0.01699 =
         0.02512    0.00927    0.01060    0.01053
CL3   4    0.233800    0.437506   -0.007075    11.00000    0.02732    0.02776 =
         0.01978    0.01190    0.01196    0.01500
CL4   4    0.282368    0.128135    0.224532    11.00000    0.02505    0.01666 =
         0.02421    0.00587    0.00877    0.01131
N     3   -0.017031    0.289529    0.222832    11.00000    0.01890    0.01701 =
         0.01985    0.00740    0.00886    0.00899
C1    1   -0.226595    0.184490    0.196064    11.00000    0.01658    0.01806 =
         0.02825    0.01037    0.01067    0.00773
AFIX  23
H1A   2   -0.317980    0.146181    0.063306    11.00000   -1.20000
H1B   2   -0.263691    0.268273    0.267035    11.00000   -1.20000
AFIX   0
C2    1   -0.256683    0.004366    0.260380    11.00000    0.02922    0.02183 =
         0.03572    0.01295    0.01789    0.00928
AFIX 137
H2A   2   -0.214490   -0.075721    0.193575    11.00000   -1.50000
H2B   2   -0.401918   -0.069984    0.235265    11.00000   -1.50000
H2C   2   -0.172980    0.043030    0.393638    11.00000   -1.50000
HKLF 4
 
REM  12SRV133 in P-1 #2
REM R1 =  0.0300 for   2463 Fo > 4sig(Fo)  and  0.0340 for all   2654 data
REM     74 parameters refined using      0 restraints
 
END  
     
WGHT      0.0270      0.1106 
REM Highest difference peak  2.359,  deepest hole -1.557,  1-sigma level  0.253
Q1    1   0.1852  0.3178  0.1727  11.00000  0.05    2.36
Q2    1   0.3041  0.4971  0.3805  11.00000  0.05    2.18
Q3    1   0.1202  0.2795  0.2378  11.00000  0.05    1.31
Q4    1   0.2458 -0.0944  0.2746  11.00000  0.05    1.26
Q5    1   0.2451  0.5443  0.3146  11.00000  0.05    1.25
Q6    1   0.2242  0.6372  0.2669  11.00000  0.05    1.21
Q7    1   0.2743  0.2747  0.2734  11.00000  0.05    1.07

REM The information below was added by Olex2.
REM
REM R1 = 0.0300 for 2463 Fo > 4sig(Fo) and n/a for all 10179 data
REM n/a parameters refined using n/a restraints
REM Highest difference peak 2.36, deepest hole -1.56
REM Mean Shift 0, Max Shift 0.

REM +++ Tabular Listing of Refinement Information +++
REM R1_all = n/a
REM R1_gt = 0.0300
REM wR_ref = 0.0665
REM GOOF = 1.117
REM Shift_max = 0
REM Shift_mean = 0
REM Reflections_all = 10179
REM Reflections_gt = 2463
REM Parameters = n/a
REM Hole = 2.36
REM Peak = -1.56
REM Flack = n/a
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W W 0.23850(3) 0.40500(3) 0.27391(2) 0.01557(7) Uani 1 1 d .
Cl1 Cl 0.34548(17) 0.41583(17) 0.59947(15) 0.0172(2) Uani 1 1 d .
Cl2 Cl 0.28460(18) 0.71694(18) 0.36966(17) 0.0203(2) Uani 1 1 d .
Cl3 Cl 0.23380(19) 0.4375(2) -0.00707(16) 0.0229(2) Uani 1 1 d .
Cl4 Cl 0.28237(18) 0.12813(18) 0.22453(16) 0.0217(2) Uani 1 1 d .
N N -0.0170(6) 0.2895(6) 0.2228(6) 0.0178(8) Uani 1 1 d .
C1 C -0.2266(7) 0.1845(7) 0.1961(7) 0.0202(9) Uani 1 1 d .
H1A H -0.3180 0.1462 0.0633 0.024 Uiso 1 1 calc R
H1B H -0.2637 0.2683 0.2670 0.024 Uiso 1 1 calc R
C2 C -0.2567(9) 0.0044(8) 0.2604(9) 0.0279(11) Uani 1 1 d .
H2A H -0.2145 -0.0757 0.1936 0.042 Uiso 1 1 calc R
H2B H -0.4019 -0.0700 0.2353 0.042 Uiso 1 1 calc R
H2C H -0.1730 0.0430 0.3936 0.042 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W 0.01614(10) 0.01513(11) 0.01780(10) 0.00775(7) 0.00810(7) 0.00748(7)
Cl1 0.0184(5) 0.0178(5) 0.0181(5) 0.0092(4) 0.0096(4) 0.0078(4)
Cl2 0.0223(5) 0.0170(6) 0.0251(5) 0.0093(4) 0.0106(4) 0.0105(4)
Cl3 0.0273(6) 0.0278(6) 0.0198(5) 0.0119(5) 0.0120(5) 0.0150(5)
Cl4 0.0250(6) 0.0167(5) 0.0242(5) 0.0059(4) 0.0088(5) 0.0113(5)
N 0.0189(18) 0.017(2) 0.0198(18) 0.0074(16) 0.0089(15) 0.0090(16)
C1 0.017(2) 0.018(2) 0.028(2) 0.010(2) 0.0107(19) 0.0077(18)
C2 0.029(3) 0.022(3) 0.036(3) 0.013(2) 0.018(2) 0.009(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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_3
Cl1 W Cl1 78.05(4) 2_666
Cl2 W Cl1 86.50(4) .
Cl2 W Cl1 82.90(4) 2_666
Cl2 W Cl4 165.19(4) .
Cl3 W Cl1 164.19(4) .
Cl3 W Cl1 86.14(4) 2_666
Cl3 W Cl2 91.43(5) .
Cl3 W Cl4 91.51(5) .
Cl4 W Cl1 82.82(4) 2_666
Cl4 W Cl1 86.74(4) .
N W Cl1 94.46(14) .
N W Cl1 172.49(14) 2_666
N W Cl2 97.33(14) .
N W Cl3 101.35(14) .
N W Cl4 96.31(15) .
W Cl1 W 101.95(4) 2_666
C1 N W 173.9(4) .
N C1 H1A 109.6 .
N C1 H1B 109.6 .
N C1 C2 110.2(4) .
H1A C1 H1B 108.1 .
C2 C1 H1A 109.6 .
C2 C1 H1B 109.6 .
C1 C2 H2A 109.5 .
C1 C2 H2B 109.5 .
C1 C2 H2C 109.5 .
H2A C2 H2B 109.5 .
H2A C2 H2C 109.5 .
H2B C2 H2C 109.5 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W Cl1 2.7155(11) 2_666
W Cl1 2.4391(11) .
W Cl2 2.3062(12) .
W Cl3 2.2837(12) .
W Cl4 2.3167(12) .
W N 1.700(4) .
Cl1 W 2.7154(11) 2_666
N C1 1.432(6) .
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C1 C2 1.525(8) .
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
