#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:09:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179742 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/38/7003888.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_7003888
loop_
_publ_author_name
'Clough, Christopher R.'
'Müller, Peter'
'Cummins, Christopher C.'
_publ_section_title
;
 6-Coordinate tungsten(vi) tris-n-isopropylanilide complexes: products
 of terminal oxo and nitrido transformations effected by main group
 electrophiles
;
_journal_issue                   33
_journal_name_full               'Dalton Transactions'
_journal_page_first              4458
_journal_page_last               4463
_journal_paper_doi               10.1039/b801037d
_journal_year                    2008
_chemical_formula_moiety         'C34 H48 Cl2 N4 O W 2(C8 H16 O2)'
_chemical_formula_sum            'C42 H64 Cl2 N4 O3 W'
_chemical_formula_weight         927.72
_chemical_name_common            W(OCN)(Cl)2(N(i-Pr)Ar)3
_chemical_name_systematic
;
?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.3600(12)
_cell_length_b                   13.3600(12)
_cell_length_c                   39.556(8)
_cell_measurement_reflns_used    3905
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.7
_cell_volume                     6114.4(15)
_computing_cell_refinement       'SAINT 5 (Bruker-AXS, 2003)'
_computing_data_collection       'SMART 5 (Bruker-AXS, 2003)'
_computing_data_reduction        'SAINT 5 (Bruker-AXS, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0493
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10803
_diffrn_reflns_theta_full        25.14
_diffrn_reflns_theta_max         25.14
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    3.008
_exptl_absorpt_correction_T_max  0.8891
_exptl_absorpt_correction_T_min  0.4972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.017
_refine_diff_density_min         -1.728
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         2442
_refine_ls_number_restraints     345
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0450
_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)+(0.0838P)²+7.7033P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                1981
_reflns_number_total             2442
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b801037d.txt
_cod_data_source_block           1-(OCN)(Cl)2
_cod_original_cell_volume        6114.5(14)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7003888
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.3333 0.6667 0.366555(12) 0.0422(2) Uani 1 3 d S . .
Cl1 Cl 0.2155(4) 0.5037(4) 0.32637(14) 0.0616(12) Uani 0.67 1 d PU A 1
O1X O 0.239(2) 0.5450(17) 0.3320(6) 0.055(5) Uani 0.33 1 d PU A 2
C1X C 0.261(2) 0.5405(18) 0.2990(6) 0.053(4) Uani 0.33 1 d PU A 2
N1X N 0.2656(18) 0.5261(19) 0.2715(5) 0.068(5) Uani 0.33 1 d PU A 2
N2 N 0.3669(4) 0.5603(4) 0.39074(15) 0.0433(13) Uani 1 1 d . A .
C1 C 0.4491(6) 0.6093(5) 0.44760(19) 0.0473(17) Uani 1 1 d . A .
H1 H 0.3734 0.5848 0.4557 0.057 Uiso 1 1 calc R . .
C2 C 0.4668(5) 0.6051(5) 0.41384(19) 0.0458(16) Uani 1 1 d . . .
C3 C 0.5402(7) 0.6487(6) 0.4703(2) 0.0551(19) Uani 1 1 d . . .
C4 C 0.5752(6) 0.6383(7) 0.4013(2) 0.062(2) Uani 1 1 d . A .
H4 H 0.5867 0.6351 0.3777 0.075 Uiso 1 1 calc R . .
C5 C 0.3168(7) 0.4322(6) 0.3845(2) 0.066(2) Uani 1 1 d . . .
H5 H 0.2399 0.4034 0.3734 0.079 Uiso 1 1 calc R A .
C6 C 0.6492(7) 0.6801(8) 0.4579(2) 0.074(3) Uani 1 1 d . A .
H6 H 0.7117 0.7043 0.4733 0.089 Uiso 1 1 calc R . .
C7 C 0.6691(7) 0.6771(9) 0.4240(3) 0.080(3) Uani 1 1 d . . .
C9 C 0.3934(8) 0.4119(8) 0.3595(3) 0.086(3) Uani 1 1 d . A .
H9A H 0.4079 0.4603 0.3394 0.128 Uiso 1 1 calc R . .
H9B H 0.3539 0.3303 0.3528 0.128 Uiso 1 1 calc R . .
H9C H 0.4670 0.4321 0.3704 0.128 Uiso 1 1 calc R . .
C10 C 0.5211(9) 0.6571(9) 0.5077(2) 0.081(3) Uani 1 1 d . A .
H10A H 0.4996 0.5832 0.5187 0.121 Uiso 1 1 calc R . .
H10B H 0.4590 0.6750 0.5108 0.121 Uiso 1 1 calc R . .
H10C H 0.5925 0.7184 0.5179 0.121 Uiso 1 1 calc R . .
C11 C 0.2959(8) 0.3656(7) 0.4170(3) 0.081(3) Uani 1 1 d . A .
H11A H 0.2591 0.3918 0.4334 0.122 Uiso 1 1 calc R . .
H11B H 0.3698 0.3787 0.4260 0.122 Uiso 1 1 calc R . .
H11C H 0.2452 0.2829 0.4126 0.122 Uiso 1 1 calc R . .
C12 C 0.7892(8) 0.7166(13) 0.4105(4) 0.146(6) Uani 1 1 d . A .
H12A H 0.8292 0.8002 0.4066 0.219 Uiso 1 1 calc R . .
H12B H 0.7836 0.6765 0.3893 0.219 Uiso 1 1 calc R . .
H12C H 0.8326 0.6987 0.4271 0.219 Uiso 1 1 calc R . .
O1S O 0.326(4) 0.655(4) 0.5671(4) 0.053(5) Uani 0.234(8) 1 d PDU B -1
C1S C 0.417(3) 0.752(3) 0.5871(8) 0.059(7) Uani 0.234(8) 1 d PDU B -1
H1S1 H 0.4059 0.8196 0.5852 0.070 Uiso 0.234(8) 1 calc PR B -1
H1S2 H 0.4935 0.7732 0.5778 0.070 Uiso 0.234(8) 1 calc PR B -1
C2S C 0.411(3) 0.717(3) 0.6266(7) 0.056(7) Uani 0.234(8) 1 d PDU B -1
H2S1 H 0.4822 0.7193 0.6352 0.067 Uiso 0.234(8) 1 calc PR B -1
H2S2 H 0.3837 0.7559 0.6421 0.067 Uiso 0.234(8) 1 calc PR B -1
C3S C 0.315(4) 0.595(4) 0.6137(9) 0.065(7) Uani 0.234(8) 1 d PDU B -1
H3S1 H 0.3498 0.5447 0.6136 0.078 Uiso 0.234(8) 1 calc PR B -1
H3S2 H 0.2537 0.5641 0.6310 0.078 Uiso 0.234(8) 1 calc PR B -1
C4S C 0.258(3) 0.580(4) 0.5807(9) 0.069(7) Uani 0.234(8) 1 d PDU B -1
H4S1 H 0.2401 0.5061 0.5699 0.083 Uiso 0.234(8) 1 calc PR B -1
H4S2 H 0.1864 0.5843 0.5827 0.083 Uiso 0.234(8) 1 calc PR B -1
O1T O 0.247(5) 0.659(6) 0.5688(15) 0.069(7) Uani 0.099(8) 1 d PDU B -2
C1T C 0.324(7) 0.717(5) 0.5984(17) 0.065(7) Uani 0.099(8) 1 d PDU B -2
H1T1 H 0.2920 0.7580 0.6118 0.078 Uiso 0.099(8) 1 calc PR B -2
H1T2 H 0.4017 0.7754 0.5905 0.078 Uiso 0.099(8) 1 calc PR B -2
C2T C 0.331(10) 0.622(8) 0.6218(14) 0.063(8) Uani 0.099(8) 1 d PDU B -2
H2T1 H 0.4102 0.6432 0.6294 0.076 Uiso 0.099(8) 1 calc PR B -2
H2T2 H 0.2746 0.5903 0.6405 0.076 Uiso 0.099(8) 1 calc PR B -2
C3T C 0.291(8) 0.549(5) 0.5882(16) 0.066(7) Uani 0.099(8) 1 d PDU B -2
H3T1 H 0.3578 0.5424 0.5802 0.079 Uiso 0.099(8) 1 calc PR B -2
H3T2 H 0.2302 0.4707 0.5946 0.079 Uiso 0.099(8) 1 calc PR B -2
C4T C 0.248(6) 0.583(7) 0.5586(13) 0.068(8) Uani 0.099(8) 1 d PDU B -2
H4T1 H 0.3005 0.6035 0.5389 0.082 Uiso 0.099(8) 1 calc PR B -2
H4T2 H 0.1694 0.5217 0.5520 0.082 Uiso 0.099(8) 1 calc PR B -2
O2S O 0.337(4) 0.594(5) 0.1534(11) 0.202(14) Uani 0.33 1 d PDU C -1
C5S C 0.394(5) 0.581(5) 0.1840(15) 0.217(15) Uani 0.33 1 d PDU C -1
H5S1 H 0.4399 0.5441 0.1777 0.260 Uiso 0.33 1 calc PR C -1
H5S2 H 0.3351 0.5311 0.2007 0.260 Uiso 0.33 1 calc PR C -1
C6S C 0.479(4) 0.707(6) 0.2006(13) 0.231(16) Uani 0.33 1 d PDU C -1
H6S1 H 0.4430 0.7308 0.2185 0.277 Uiso 0.33 1 calc PR C -1
H6S2 H 0.5563 0.7214 0.2072 0.277 Uiso 0.33 1 calc PR C -1
C7S C 0.471(4) 0.748(5) 0.1639(14) 0.205(15) Uani 0.33 1 d PDU C -1
H7S1 H 0.4777 0.8252 0.1662 0.246 Uiso 0.33 1 calc PR C -1
H7S2 H 0.5408 0.7605 0.1516 0.246 Uiso 0.33 1 calc PR C -1
C8S C 0.371(4) 0.679(7) 0.1417(12) 0.200(16) Uani 0.33 1 d PDU C -1
H8S1 H 0.3145 0.7060 0.1423 0.240 Uiso 0.33 1 calc PR C -1
H8S2 H 0.3954 0.6790 0.1180 0.240 Uiso 0.33 1 calc PR C -1
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'
O O 0.0106 0.0060 '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_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 W1 N2 97.8(2) 3_565 . ?
N2 W1 N2 97.8(2) 3_565 2_665 ?
N2 W1 N2 97.8(2) . 2_665 ?
N2 W1 O1X 91.4(7) 3_565 3_565 ?
N2 W1 O1X 166.7(7) . 3_565 ?
N2 W1 O1X 90.3(8) 2_665 3_565 ?
N2 W1 O1X 90.3(8) 3_565 . ?
N2 W1 O1X 91.4(7) . . ?
N2 W1 O1X 166.7(7) 2_665 . ?
O1X W1 O1X 79.0(10) 3_565 . ?
N2 W1 O1X 166.7(7) 3_565 2_665 ?
N2 W1 O1X 90.3(8) . 2_665 ?
N2 W1 O1X 91.4(7) 2_665 2_665 ?
O1X W1 O1X 79.0(10) 3_565 2_665 ?
O1X W1 O1X 79.0(10) . 2_665 ?
N2 W1 Cl1 87.2(2) 3_565 3_565 ?
N2 W1 Cl1 170.1(2) . 3_565 ?
N2 W1 Cl1 89.9(2) 2_665 3_565 ?
O1X W1 Cl1 4.3(7) 3_565 3_565 ?
O1X W1 Cl1 80.0(7) . 3_565 ?
O1X W1 Cl1 83.2(8) 2_665 3_565 ?
N2 W1 Cl1 89.9(2) 3_565 . ?
N2 W1 Cl1 87.2(2) . . ?
N2 W1 Cl1 170.1(2) 2_665 . ?
O1X W1 Cl1 83.2(8) 3_565 . ?
O1X W1 Cl1 4.3(8) . . ?
O1X W1 Cl1 80.0(7) 2_665 . ?
Cl1 W1 Cl1 84.26(19) 3_565 . ?
N2 W1 Cl1 170.1(2) 3_565 2_665 ?
N2 W1 Cl1 89.9(2) . 2_665 ?
N2 W1 Cl1 87.2(2) 2_665 2_665 ?
O1X W1 Cl1 80.0(7) 3_565 2_665 ?
O1X W1 Cl1 83.2(8) . 2_665 ?
O1X W1 Cl1 4.3(7) 2_665 2_665 ?
Cl1 W1 Cl1 84.26(19) 3_565 2_665 ?
Cl1 W1 Cl1 84.26(19) . 2_665 ?
C1X O1X W1 129.3(19) . . ?
N1X C1X O1X 172(3) . . ?
C2 N2 C5 111.1(5) . . ?
C2 N2 W1 120.1(4) . . ?
C5 N2 W1 127.8(4) . . ?
C2 C1 C3 120.8(7) . . ?
C1 C2 C4 121.1(6) . . ?
C1 C2 N2 118.9(6) . . ?
C4 C2 N2 120.0(7) . . ?
C1 C3 C6 118.4(7) . . ?
C1 C3 C10 120.8(7) . . ?
C6 C3 C10 120.8(7) . . ?
C2 C4 C7 119.1(8) . . ?
C11 C5 N2 112.0(7) . . ?
C11 C5 C9 112.7(7) . . ?
N2 C5 C9 110.3(7) . . ?
C7 C6 C3 121.7(7) . . ?
C6 C7 C4 118.8(8) . . ?
C6 C7 C12 121.4(9) . . ?
C4 C7 C12 119.8(9) . . ?
C4S O1S C1S 118(2) . . ?
O1S C1S C2S 111(2) . . ?
C3S C2S C1S 83.0(19) . . ?
C4S C3S C2S 122(3) . . ?
O1S C4S C3S 100(3) . . ?
C4T O1T C1T 117(3) . . ?
O1T C1T C2T 109(3) . . ?
C3T C2T C1T 82(2) . . ?
C4T C3T C2T 123(3) . . ?
O1T C4T C3T 100(3) . . ?
C8S O2S C5S 119(2) . . ?
O2S C5S C6S 110(2) . . ?
C7S C6S C5S 82(2) . . ?
C8S C7S C6S 122(3) . . ?
O2S C8S C7S 100(3) . . ?
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
W1 N2 1.943(5) 3_565 ?
W1 N2 1.943(5) . ?
W1 N2 1.943(5) 2_665 ?
W1 O1X 2.01(2) 3_565 ?
W1 O1X 2.01(2) . ?
W1 O1X 2.01(2) 2_665 ?
W1 Cl1 2.513(4) 3_565 ?
W1 Cl1 2.513(4) . ?
W1 Cl1 2.513(4) 2_665 ?
O1X C1X 1.35(4) . ?
C1X N1X 1.11(3) . ?
N2 C2 1.475(8) . ?
N2 C5 1.514(8) . ?
C1 C2 1.362(10) . ?
C1 C3 1.386(10) . ?
C2 C4 1.378(10) . ?
C3 C6 1.388(11) . ?
C3 C10 1.516(12) . ?
C4 C7 1.413(10) . ?
C5 C11 1.507(12) . ?
C5 C9 1.541(12) . ?
C6 C7 1.371(14) . ?
C7 C12 1.513(13) . ?
O1S C4S 1.10(5) . ?
O1S C1S 1.49(4) . ?
C1S C2S 1.62(3) . ?
C2S C3S 1.57(5) . ?
C3S C4S 1.48(4) . ?
O1T C4T 1.10(5) . ?
O1T C1T 1.49(4) . ?
C1T C2T 1.62(3) . ?
C2T C3T 1.57(5) . ?
C3T C4T 1.48(4) . ?
O2S C8S 1.09(5) . ?
O2S C5S 1.49(4) . ?
C5S C6S 1.63(3) . ?
C6S C7S 1.57(5) . ?
C7S C8S 1.48(4) . ?
