#------------------------------------------------------------------------------
#$Date: 2019-11-10 07:54:14 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225918 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/58/4515802.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_4515802
loop_
_publ_author_name
'Messinis, Antonis M.'
'Batsanov, Andrei S.'
'Wright, William R. H.'
'Howard, Judith A. K.'
'Hanton, Martin J.'
'Dyer, Philip W.'
_publ_section_title
;
 Bis(Imido) Tungsten Complexes: Efficient Precatalysts for the Homogeneous
 Dimerization of Ethylene
;
_journal_issue                   12
_journal_name_full               'ACS Catalysis'
_journal_page_first              11249
_journal_paper_doi               10.1021/acscatal.8b02202
_journal_volume                  8
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H43 Cl2 N2 P W'
_chemical_formula_sum            'C27 H43 Cl2 N2 P W'
_chemical_formula_weight         681.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-10-24
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5486(9)
_cell_length_b                   16.4202(14)
_cell_length_c                   17.0860(13)
_cell_measurement_reflns_used    9882
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      33.85
_cell_measurement_theta_min      2.29
_cell_volume                     2959.5(4)
_computing_cell_refinement       'SAINT v7.46A (Bruker, 2008)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.46A (Bruker, 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0463
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            68981
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         1.720
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35.0
_diffrn_source_power             1.75
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.155
_exptl_absorpt_correction_T_max  0.7219
_exptl_absorpt_correction_T_min  0.3226
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0845 before and 0.0771 after correction.
The Ratio of minimum to maximum transmission is 0.4469.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.529
_exptl_crystal_description       needle
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         4.336
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.149
_refine_ls_abs_structure_details
;
 Flack x determined using 4767 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). By 
 classical fit to all intensities, x = -0.018(7). Hooft y = -0.014(4).
;
_refine_ls_abs_structure_Flack   -0.016(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         12654
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0334
_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)+(0.0322P)²+0.1589P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.953
_reflns_number_gt                11469
_reflns_number_total             12654
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            W-bisimido.cif
_cod_data_source_block           6_11srv202
_cod_database_code               4515802
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.760
_shelx_estimated_absorpt_t_min   0.287
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Uiso(H8A)=Uiso(H8B)=Uiso(H8C)=FVAR(1)
 Uiso(H9A)=Uiso(H9B)=Uiso(H9C)=FVAR(2)
 Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(3)
 Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(4)
 Uiso(H20A)=Uiso(H20B)=Uiso(H20C)=FVAR(5)
 Uiso(H21A)=Uiso(H21B)=Uiso(H21C)=FVAR(6)
 Uiso(H23A)=Uiso(H23B)=Uiso(H23C)=FVAR(7)
 Uiso(H24A)=Uiso(H24B)=Uiso(H24C)=FVAR(8)
 Uiso(H25A)=Uiso(H25B)=Uiso(H25C)=FVAR(9)
 Uiso(H26A)=Uiso(H26B)=Uiso(H26C)=FVAR(10)
 Uiso(H27A)=Uiso(H27B)=Uiso(H27C)=FVAR(11)
3.a Riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C10(H10), C15(H15), C16(H16), C17(H17),
 C19(H19), C22(H22)
3.b Rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
W W 0.07134(2) 0.48699(2) 0.65738(2) 0.01352(4) Uani 1 1 d .
Cl1 Cl -0.01500(11) 0.35945(7) 0.61972(7) 0.0247(2) Uani 1 1 d .
Cl2 Cl -0.06041(11) 0.46558(8) 0.77267(6) 0.0273(2) Uani 1 1 d .
P P 0.04318(12) 0.63024(8) 0.70835(7) 0.0212(2) Uani 1 1 d .
N1 N 0.2333(3) 0.4683(2) 0.6751(2) 0.0156(6) Uani 1 1 d .
N2 N 0.0500(3) 0.5334(2) 0.5651(2) 0.0155(6) Uani 1 1 d .
C1 C 0.3647(4) 0.4566(2) 0.6670(2) 0.0164(7) Uani 1 1 d .
C2 C 0.4086(4) 0.3873(3) 0.6259(2) 0.0189(8) Uani 1 1 d .
C3 C 0.5395(4) 0.3742(4) 0.6235(3) 0.0274(10) Uani 1 1 d .
H3 H 0.571098 0.327975 0.596337 0.033 Uiso 1 1 d R
C4 C 0.6242(4) 0.4260(3) 0.6593(3) 0.0313(11) Uani 1 1 d .
H4 H 0.712519 0.414915 0.657501 0.038 Uiso 1 1 d R
C5 C 0.5797(4) 0.4942(3) 0.6977(3) 0.0275(10) Uani 1 1 d .
H5 H 0.638708 0.529942 0.721897 0.033 Uiso 1 1 d R
C6 C 0.4501(4) 0.5120(3) 0.7022(2) 0.0207(8) Uani 1 1 d .
C7 C 0.3172(5) 0.3280(3) 0.5886(3) 0.0210(8) Uani 1 1 d .
H7 H 0.241303 0.359622 0.570965 0.025 Uiso 1 1 d R
C8 C 0.2726(5) 0.2667(3) 0.6504(3) 0.0278(10) Uani 1 1 d .
H8A H 0.344750 0.233583 0.667660 0.040(11) Uiso 1 1 d GR
H8B H 0.207490 0.231262 0.627839 0.040(11) Uiso 1 1 d GR
H8C H 0.237248 0.295993 0.695399 0.040(11) Uiso 1 1 d GR
C9 C 0.3709(6) 0.2839(4) 0.5172(3) 0.0348(12) Uani 1 1 d .
H9A H 0.413302 0.323158 0.482958 0.047(11) Uiso 1 1 d GR
H9B H 0.301802 0.257348 0.488618 0.047(11) Uiso 1 1 d GR
H9C H 0.432122 0.242638 0.534428 0.047(11) Uiso 1 1 d GR
C10 C 0.4047(5) 0.5880(3) 0.7445(3) 0.0256(10) Uani 1 1 d .
H10 H 0.310472 0.590791 0.738751 0.031 Uiso 1 1 d R
C11 C 0.4352(6) 0.5852(3) 0.8326(3) 0.0346(11) Uani 1 1 d .
H11A H 0.397934 0.536072 0.855674 0.040(10) Uiso 1 1 d GR
H11B H 0.399667 0.633492 0.858234 0.040(10) Uiso 1 1 d GR
H11C H 0.527305 0.584320 0.840034 0.040(10) Uiso 1 1 d GR
C12 C 0.4607(6) 0.6651(3) 0.7075(4) 0.0371(13) Uani 1 1 d .
H12A H 0.553315 0.663664 0.712010 0.048(12) Uiso 1 1 d GR
H12B H 0.427866 0.713134 0.734812 0.048(12) Uiso 1 1 d GR
H12C H 0.436754 0.667595 0.652161 0.048(12) Uiso 1 1 d GR
C13 C 0.0362(4) 0.5708(3) 0.4928(2) 0.0153(7) Uani 1 1 d .
C14 C -0.0852(4) 0.5730(3) 0.4581(2) 0.0177(7) Uani 1 1 d .
C15 C -0.0954(4) 0.6063(3) 0.3832(3) 0.0227(9) Uani 1 1 d .
H15 H -0.175787 0.607715 0.358064 0.027 Uiso 1 1 d R
C16 C 0.0091(4) 0.6371(3) 0.3451(3) 0.0240(8) Uani 1 1 d .
H16 H -0.000061 0.658998 0.293940 0.029 Uiso 1 1 d R
C17 C 0.1276(5) 0.6366(3) 0.3803(3) 0.0224(9) Uani 1 1 d .
H17 H 0.198173 0.659153 0.353432 0.027 Uiso 1 1 d R
C18 C 0.1442(4) 0.6034(3) 0.4544(2) 0.0171(7) Uani 1 1 d .
C19 C -0.2008(4) 0.5362(3) 0.4977(3) 0.0209(8) Uani 1 1 d .
H19 H -0.177771 0.524982 0.553436 0.025 Uiso 1 1 d R
C20 C -0.2349(5) 0.4546(3) 0.4592(3) 0.0286(10) Uani 1 1 d .
H20A H -0.256340 0.463593 0.404089 0.038(11) Uiso 1 1 d GR
H20B H -0.307682 0.430564 0.486308 0.038(11) Uiso 1 1 d GR
H20C H -0.162252 0.417543 0.462710 0.038(11) Uiso 1 1 d GR
C21 C -0.3154(5) 0.5924(4) 0.4979(3) 0.0294(11) Uani 1 1 d .
H21A H -0.290711 0.645819 0.518389 0.033(10) Uiso 1 1 d GR
H21B H -0.381850 0.569029 0.531124 0.033(10) Uiso 1 1 d GR
H21C H -0.347475 0.598445 0.444392 0.033(10) Uiso 1 1 d GR
C22 C 0.2753(4) 0.5955(3) 0.4904(3) 0.0197(8) Uani 1 1 d .
H22 H 0.264790 0.590855 0.548416 0.024 Uiso 1 1 d R
C23 C 0.3372(4) 0.5171(3) 0.4612(3) 0.0263(9) Uani 1 1 d .
H23A H 0.357318 0.522619 0.405413 0.045(11) Uiso 1 1 d GR
H23B H 0.278731 0.471449 0.468645 0.045(11) Uiso 1 1 d GR
H23C H 0.415351 0.507090 0.490663 0.045(11) Uiso 1 1 d GR
C24 C 0.3595(5) 0.6698(3) 0.4740(4) 0.0301(11) Uani 1 1 d .
H24A H 0.439036 0.664599 0.503172 0.033(10) Uiso 1 1 d GR
H24B H 0.315316 0.719439 0.490410 0.033(10) Uiso 1 1 d GR
H24C H 0.377858 0.672748 0.417791 0.033(10) Uiso 1 1 d GR
C25 C 0.0730(6) 0.6499(3) 0.8109(3) 0.0316(10) Uani 1 1 d .
H25A H 0.014578 0.617447 0.842836 0.051(12) Uiso 1 1 d GR
H25B H 0.059879 0.707857 0.821766 0.051(12) Uiso 1 1 d GR
H25C H 0.160508 0.634946 0.823546 0.051(12) Uiso 1 1 d GR
C26 C 0.1268(5) 0.7092(3) 0.6560(4) 0.0294(10) Uani 1 1 d .
H26A H 0.218199 0.702680 0.663939 0.056(13) Uiso 1 1 d GR
H26B H 0.100101 0.762621 0.675573 0.056(13) Uiso 1 1 d GR
H26C H 0.107406 0.705193 0.600051 0.056(13) Uiso 1 1 d GR
C27 C -0.1218(5) 0.6582(4) 0.6938(3) 0.0306(11) Uani 1 1 d .
H27A H -0.143969 0.651840 0.638423 0.024(9) Uiso 1 1 d GR
H27B H -0.134457 0.715053 0.709480 0.024(9) Uiso 1 1 d GR
H27C H -0.176038 0.622834 0.725624 0.024(9) Uiso 1 1 d GR
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 1.00 1.00 0.0350
0.00 -1.00 -1.00 0.0350
0.00 -1.00 1.00 0.0400
0.00 1.00 -1.00 0.0400
1.00 0.00 -1.00 0.1800
-3.00 1.00 -4.00 0.1300
-1.00 0.00 0.00 0.1800
1.00 0.00 0.00 0.2200
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl1 W Cl2 82.70(4)
Cl1 W P 150.50(4)
Cl2 W P 77.79(4)
N1 W Cl1 105.37(12)
N1 W Cl2 112.92(12)
N1 W P 102.54(12)
N1 W N2 110.61(16)
N2 W Cl1 95.15(12)
N2 W Cl2 135.36(11)
N2 W P 83.74(12)
C25 P W 118.66(18)
C25 P C27 104.7(3)
C26 P W 116.15(18)
C26 P C25 105.5(3)
C26 P C27 102.6(3)
C27 P W 107.51(19)
C1 N1 W 164.4(3)
C13 N2 W 178.6(3)
N1 C1 C2 118.8(4)
N1 C1 C6 119.9(4)
C6 C1 C2 121.3(4)
C1 C2 C7 121.2(4)
C3 C2 C1 117.5(4)
C3 C2 C7 121.2(4)
C4 C3 C2 122.2(5)
C3 C4 C5 119.5(4)
C4 C5 C6 121.8(5)
C1 C6 C10 122.0(4)
C5 C6 C1 117.7(5)
C5 C6 C10 120.3(4)
C2 C7 C8 109.2(4)
C2 C7 C9 113.9(4)
C9 C7 C8 110.6(4)
C6 C10 C11 112.0(4)
C6 C10 C12 111.1(4)
C12 C10 C11 110.3(4)
N2 C13 C14 118.8(4)
N2 C13 C18 119.6(4)
C14 C13 C18 121.6(4)
C13 C14 C19 122.0(4)
C15 C14 C13 117.8(4)
C15 C14 C19 120.1(4)
C16 C15 C14 121.0(4)
C15 C16 C17 121.0(4)
C16 C17 C18 120.7(4)
C13 C18 C22 120.8(4)
C17 C18 C13 117.9(4)
C17 C18 C22 121.1(4)
C14 C19 C20 110.1(4)
C14 C19 C21 113.4(4)
C21 C19 C20 110.1(4)
C18 C22 C23 109.2(4)
C18 C22 C24 112.7(4)
C23 C22 C24 111.2(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W Cl1 2.3727(12)
W Cl2 2.4363(11)
W P 2.5257(12)
W N1 1.762(3)
W N2 1.765(3)
P C25 1.809(5)
P C26 1.805(5)
P C27 1.817(5)
N1 C1 1.406(5)
N2 C13 1.387(5)
C1 C2 1.415(6)
C1 C6 1.414(6)
C2 C3 1.398(6)
C2 C7 1.512(6)
C3 C4 1.376(8)
C4 C5 1.380(8)
C5 C6 1.401(6)
C6 C10 1.519(7)
C7 C8 1.533(7)
C7 C9 1.527(7)
C10 C11 1.540(7)
C10 C12 1.533(7)
C13 C14 1.412(6)
C13 C18 1.420(6)
C14 C15 1.396(6)
C14 C19 1.520(6)
C15 C16 1.377(7)
C16 C17 1.387(7)
C17 C18 1.390(6)
C18 C22 1.519(6)
C19 C20 1.536(7)
C19 C21 1.520(7)
C22 C23 1.528(7)
C22 C24 1.535(7)
