#------------------------------------------------------------------------------
#$Date: 2019-11-10 07:47:08 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225905 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515789.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_4515789
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         'C15 H26 Al Cl4 N W'
_chemical_formula_sum            'C15 H26 Al Cl4 N W'
_chemical_formula_weight         573.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-25
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.616(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0824(5)
_cell_length_b                   16.3429(10)
_cell_length_c                   13.3029(7)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    120
_cell_measurement_theta_max      34.93
_cell_measurement_theta_min      2.38
_cell_volume                     2177.4(2)
_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 2014/7 multi-CPU version (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_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 0.967
_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  0.0224
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50007
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        32.500
_diffrn_reflns_theta_max         34.982
_diffrn_reflns_theta_min         1.982
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.833
_exptl_absorpt_correction_T_max  0.4370
_exptl_absorpt_correction_T_min  0.3573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; SADABS-2009/1 (Bruker,2010) was used for absorption correction. wR2(int) 
 was 0.0618 before and 0.0375 after correction. The Ratio of minimum to maximum 
 transmission is 0.8176. The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.505
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         9270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0132P)²+1.1294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0342
_refine_ls_wR_factor_ref         0.0351
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8368
_reflns_number_total             9270
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs8b02201_si_002.cif
_cod_data_source_block           7
_cod_database_code               4515789
_shelx_shelxl_version_number     2014/7
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Uiso(H14A)=Uiso(H14B)=Uiso(H14C)=FVAR(1)
 Uiso(H15A)=Uiso(H15B)=Uiso(H15C)=FVAR(2)
 Uiso(H3AA)=Uiso(H3AB)=Uiso(H3AC)=Uiso(H3BD)=Uiso(H3BE)=Uiso(H3BF)=FVAR(3)
 Uiso(H2A)=Uiso(H2B)=Uiso(H2C)=FVAR(4)
 Uiso(H1A)=Uiso(H1B)=Uiso(H1C)=FVAR(5)
 Uiso(H12A)=Uiso(H12B)=Uiso(H12C)=FVAR(6)
 Uiso(H11A)=Uiso(H11B)=Uiso(H11C)=FVAR(7)
 Fixed Sof: H3AA(0.67) H3AB(0.67) H3AC(0.67) H3BD(0.33) H3BE(0.33) H3BF(0.33)
3.a Riding coordinates:
 C3(H3AA,H3AB,H3AC,H3BD,H3BE,H3BF), C6(H6), C7(H7), C8(H8), C10(H10), C13(H13)
3.b Rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.69391(2) 0.46937(2) 0.75434(2) 0.01524(2) Uani 1 1 d . . . .
Cl1 Cl 0.66381(4) 0.37403(2) 0.91136(2) 0.02259(6) Uani 1 1 d . . . .
Cl2 Cl 0.98355(5) 0.38123(4) 1.04557(4) 0.04352(11) Uani 1 1 d . . . .
Cl3 Cl 0.72418(6) 0.50389(3) 1.11766(3) 0.03984(10) Uani 1 1 d . . . .
Cl4 Cl 0.71329(6) 0.29170(3) 1.14974(3) 0.04450(12) Uani 1 1 d . . . .
Al Al 0.77885(5) 0.38895(3) 1.06334(3) 0.02290(9) Uani 1 1 d . . . .
N N 0.71536(11) 0.52039(7) 0.64392(8) 0.01677(19) Uani 1 1 d . . . .
C1 C 0.52775(14) 0.40116(9) 0.69578(11) 0.0228(3) Uani 1 1 d . . . .
H1A H 0.5501 0.3428 0.6987 0.051(4) Uiso 1 1 d GR . . .
H1B H 0.5013 0.4171 0.6253 0.051(4) Uiso 1 1 d GR . . .
H1C H 0.4538 0.4116 0.7357 0.051(4) Uiso 1 1 d GR . . .
C2 C 0.88528(14) 0.41811(11) 0.76940(12) 0.0267(3) Uani 1 1 d . . . .
H2A H 0.9337 0.4348 0.8343 0.062(5) Uiso 1 1 d GR . . .
H2B H 0.9336 0.4372 0.7140 0.062(5) Uiso 1 1 d GR . . .
H2C H 0.8782 0.3583 0.7669 0.062(5) Uiso 1 1 d GR . . .
C3 C 0.65660(17) 0.56821(9) 0.84645(11) 0.0269(3) Uani 1 1 d . . . .
H3AA H 0.5818 0.5549 0.8845 0.046(5) Uiso 0.67 1 d R P A 1
H3AB H 0.6341 0.6166 0.8043 0.046(5) Uiso 0.67 1 d R P A 1
H3AC H 0.7364 0.5796 0.8938 0.046(5) Uiso 0.67 1 d R P A 1
H3BD H 0.6702 0.5566 0.9091 0.046(5) Uiso 0.33 1 d R P B 2
H3BE H 0.7181 0.6117 0.8312 0.046(5) Uiso 0.33 1 d R P B 2
H3BF H 0.5645 0.5853 0.8250 0.046(5) Uiso 0.33 1 d R P B 2
C4 C 0.74580(12) 0.55136(8) 0.55158(9) 0.0156(2) Uani 1 1 d . . . .
C5 C 0.75422(13) 0.63709(8) 0.53953(10) 0.0170(2) Uani 1 1 d . . . .
C6 C 0.78840(14) 0.66631(8) 0.44767(10) 0.0204(2) Uani 1 1 d . . . .
H6 H 0.7938 0.7236 0.4370 0.025 Uiso 1 1 d R . . .
C7 C 0.81476(14) 0.61263(9) 0.37151(10) 0.0220(3) Uani 1 1 d . . . .
H7 H 0.8390 0.6336 0.3096 0.026 Uiso 1 1 d R . . .
C8 C 0.80610(14) 0.52896(9) 0.38487(10) 0.0202(2) Uani 1 1 d . . . .
H8 H 0.8252 0.4933 0.3320 0.024 Uiso 1 1 d R . . .
C9 C 0.76986(13) 0.49579(8) 0.47447(9) 0.0169(2) Uani 1 1 d . . . .
C10 C 0.73226(14) 0.69331(8) 0.62642(11) 0.0207(2) Uani 1 1 d . . . .
H10 H 0.6612 0.6685 0.6633 0.025 Uiso 1 1 d R . . .
C11 C 0.68591(18) 0.77908(9) 0.59243(13) 0.0305(3) Uani 1 1 d . . . .
H11A H 0.7588 0.8077 0.5645 0.038(3) Uiso 1 1 d GR . . .
H11B H 0.6602 0.8096 0.6506 0.038(3) Uiso 1 1 d GR . . .
H11C H 0.6090 0.7748 0.5405 0.038(3) Uiso 1 1 d GR . . .
C12 C 0.86055(17) 0.69812(10) 0.70041(12) 0.0290(3) Uani 1 1 d . . . .
H12A H 0.8914 0.6427 0.7189 0.034(3) Uiso 1 1 d GR . . .
H12B H 0.8425 0.7278 0.7614 0.034(3) Uiso 1 1 d GR . . .
H12C H 0.9296 0.7270 0.6682 0.034(3) Uiso 1 1 d GR . . .
C13 C 0.75059(13) 0.40428(8) 0.48367(10) 0.0192(2) Uani 1 1 d . . . .
H13 H 0.7497 0.3909 0.5569 0.023 Uiso 1 1 d R . . .
C14 C 0.61564(15) 0.37954(10) 0.42765(13) 0.0280(3) Uani 1 1 d . . . .
H14A H 0.5445 0.4109 0.4541 0.038(3) Uiso 1 1 d GR . . .
H14B H 0.6008 0.3209 0.4375 0.038(3) Uiso 1 1 d GR . . .
H14C H 0.6150 0.3909 0.3552 0.038(3) Uiso 1 1 d GR . . .
C15 C 0.86281(16) 0.35553(10) 0.44450(13) 0.0287(3) Uani 1 1 d . . . .
H15A H 0.8588 0.3625 0.3710 0.039(3) Uiso 1 1 d GR . . .
H15B H 0.8528 0.2975 0.4603 0.039(3) Uiso 1 1 d GR . . .
H15C H 0.9490 0.3754 0.4769 0.039(3) 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'
Al Al 0.0645 0.0514 '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'
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
N W Cl1 172.93(4)
N W C1 96.57(5)
N W C2 94.03(6)
N W C3 100.05(6)
C1 W Cl1 79.65(4)
C1 W C2 120.91(6)
C1 W C3 116.18(6)
C2 W Cl1 82.95(4)
C3 W Cl1 87.00(4)
C3 W C2 118.70(7)
Al Cl1 W 123.807(18)
Cl2 Al Cl1 107.83(3)
Cl2 Al Cl3 112.94(3)
Cl2 Al Cl4 112.83(3)
Cl3 Al Cl1 106.23(3)
Cl3 Al Cl4 111.92(3)
Cl4 Al Cl1 104.42(3)
C4 N W 170.94(10)
N C4 C5 118.78(11)
N C4 C9 118.69(11)
C9 C4 C5 122.51(12)
C4 C5 C10 119.95(11)
C6 C5 C4 117.63(12)
C6 C5 C10 122.36(12)
C7 C6 C5 120.75(12)
C8 C7 C6 120.70(12)
C7 C8 C9 121.36(13)
C4 C9 C13 122.82(11)
C8 C9 C4 117.02(12)
C8 C9 C13 120.07(12)
C5 C10 C11 113.41(12)
C5 C10 C12 109.54(11)
C11 C10 C12 110.42(13)
C9 C13 C14 109.70(11)
C9 C13 C15 112.41(12)
C15 C13 C14 110.44(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W Cl1 2.6512(3)
W N 1.7243(11)
W C1 2.0869(14)
W C2 2.0918(14)
W C3 2.0878(14)
Cl1 Al 2.2253(6)
Cl2 Al 2.1080(7)
Cl3 Al 2.1087(6)
Cl4 Al 2.1116(6)
N C4 1.3951(16)
C4 C5 1.4139(18)
C4 C9 1.4118(18)
C5 C6 1.3919(18)
C5 C10 1.5128(19)
C6 C7 1.389(2)
C7 C8 1.383(2)
C8 C9 1.3959(18)
C9 C13 1.5148(19)
C10 C11 1.529(2)
C10 C12 1.535(2)
C13 C14 1.529(2)
C13 C15 1.524(2)
