#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/01/7010141.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_7010141
loop_
_publ_author_name
'Nielson, Alastair J.'
'Glenny, Mark W.'
'Rickard, Clifton E. F.'
'Waters, Joyce M.'
_publ_section_title
;
 Regiospecific influences of phenyl ring substituents in monoimido
 complexes of tantalum and tungsten and bis imido complexes of
 molybdenum
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4569
_journal_paper_doi               10.1039/b006420n
_journal_year                    2000
_chemical_formula_moiety         '[W Cl2 (N C6H4 CMe3-2)(P Me3)3]'
_chemical_formula_sum            'C22.5 H43.5 Cl2 N P3 W'
_chemical_formula_weight         675.74
_chemical_name_systematic        '[W Cl2 (N C6H4 CMe3-2)(P Me3)3]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.39
_cell_angle_beta                 94.6940(10)
_cell_angle_gamma                116.93
_cell_formula_units_Z            2
_cell_length_a                   8.688
_cell_length_b                   9.43090(10)
_cell_length_c                   19.9949(3)
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1453.97(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'Siemens SMART (Siemens, 1995)'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Siemens SMART'
_diffrn_measurement_method       'area detectorω 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6288
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.332
_exptl_absorpt_correction_T_max  0.5822
_exptl_absorpt_correction_T_min  0.2303
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             677
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.059
_refine_diff_density_min         -1.051
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         6288
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0327P)²+3.6560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                6046
_reflns_number_total             6288
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006420n.txt
_cod_data_source_block           mg188
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+3.6560P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+3.6560P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1453.94(3)
_cod_original_sg_symbol_H-M      P(1-bar)
_cod_original_formula_sum        'C22.50 H43.50 Cl2 N P3 W'
_cod_database_code               7010141
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
W W 0.581684(17) 0.679488(15) 0.689010(6) 0.01818(5) Uani 1 d . . .
Cl1 Cl 0.60630(13) 0.51262(11) 0.59699(5) 0.03016(19) Uani 1 d . . .
Cl2 Cl 0.89145(12) 0.74184(12) 0.72224(5) 0.03068(19) Uani 1 d . . .
P1 P 0.69929(13) 0.89347(11) 0.60682(5) 0.02538(19) Uani 1 d . . .
P2 P 0.50286(13) 0.42790(12) 0.74994(5) 0.0262(2) Uani 1 d . . .
P3 P 0.27793(12) 0.58865(12) 0.64009(5) 0.02418(19) Uani 1 d . . .
N N 0.5541(4) 0.7933(4) 0.75344(14) 0.0203(6) Uani 1 d . . .
C1 C 0.5102(5) 0.8754(4) 0.80155(17) 0.0209(7) Uani 1 d . . .
C2 C 0.3403(5) 0.8592(5) 0.7922(2) 0.0274(8) Uani 1 d . . .
H2 H 0.2668 0.7991 0.7545 0.033 Uiso 1 calc R . .
C3 C 0.2785(5) 0.9296(5) 0.8371(2) 0.0326(9) Uani 1 d . . .
H3 H 0.1648 0.9174 0.8298 0.039 Uiso 1 calc R . .
C4 C 0.3860(6) 1.0179(5) 0.8927(2) 0.0325(9) Uani 1 d . . .
H4 H 0.3452 1.0646 0.9239 0.039 Uiso 1 calc R . .
C5 C 0.5540(6) 1.0369(5) 0.90201(19) 0.0294(8) Uani 1 d . . .
H5 H 0.6251 1.0982 0.9399 0.035 Uiso 1 calc R . .
C6 C 0.6241(5) 0.9699(4) 0.85816(17) 0.0220(7) Uani 1 d . . .
C7 C 0.8119(5) 0.9985(4) 0.87191(18) 0.0243(7) Uani 1 d . . .
C8 C 0.9138(5) 1.0789(5) 0.8114(2) 0.0296(8) Uani 1 d . . .
H8C H 0.8642 1.0079 0.7716 0.044 Uiso 1 calc R . .
H8B H 1.0343 1.1019 0.8210 0.044 Uiso 1 calc R . .
H8A H 0.9068 1.1773 0.8035 0.044 Uiso 1 calc R . .
C9 C 0.8144(5) 0.8387(5) 0.8855(2) 0.0287(8) Uani 1 d . . .
H9C H 0.7491 0.7917 0.9234 0.043 Uiso 1 calc R . .
H9B H 0.9332 0.8570 0.8955 0.043 Uiso 1 calc R . .
H9A H 0.7624 0.7670 0.8460 0.043 Uiso 1 calc R . .
C10 C 0.9075(6) 1.1118(6) 0.9341(2) 0.0386(10) Uani 1 d . . .
H10C H 0.8462 1.0676 0.9733 0.058 Uiso 1 calc R . .
H10B H 0.9115 1.2149 0.9267 0.058 Uiso 1 calc R . .
H10A H 1.0246 1.1239 0.9415 0.058 Uiso 1 calc R . .
C11 C 0.9305(6) 0.9723(7) 0.5962(3) 0.0503(13) Uani 1 d . . .
H11C H 0.9649 1.0608 0.5668 0.076 Uiso 1 calc R . .
H11B H 0.9518 0.8893 0.5765 0.076 Uiso 1 calc R . .
H11A H 0.9972 1.0085 0.6396 0.076 Uiso 1 calc R . .
C12 C 0.6102(6) 0.8491(5) 0.5191(2) 0.0364(9) Uani 1 d . . .
H12C H 0.6764 0.9388 0.4927 0.055 Uiso 1 calc R . .
H12B H 0.4900 0.8294 0.5155 0.055 Uiso 1 calc R . .
H12A H 0.6166 0.7553 0.5023 0.055 Uiso 1 calc R . .
C13 C 0.6797(7) 1.0722(5) 0.6290(2) 0.0443(11) Uani 1 d . . .
H13C H 0.7284 1.1505 0.5956 0.066 Uiso 1 calc R . .
H13B H 0.7421 1.1160 0.6727 0.066 Uiso 1 calc R . .
H13A H 0.5583 1.0453 0.6306 0.066 Uiso 1 calc R . .
C14 C 0.3459(7) 0.2401(5) 0.7067(2) 0.0416(10) Uani 1 d . . .
H14C H 0.3411 0.1519 0.7326 0.062 Uiso 1 calc R . .
H14B H 0.3811 0.2321 0.6625 0.062 Uiso 1 calc R . .
H14A H 0.2323 0.2368 0.7019 0.062 Uiso 1 calc R . .
C15 C 0.4116(6) 0.4257(6) 0.8292(2) 0.0388(10) Uani 1 d . . .
H15C H 0.3851 0.3257 0.8501 0.058 Uiso 1 calc R . .
H15B H 0.3062 0.4369 0.8207 0.058 Uiso 1 calc R . .
H15A H 0.4950 0.5132 0.8590 0.058 Uiso 1 calc R . .
C16 C 0.6803(7) 0.3788(6) 0.7746(3) 0.0460(11) Uani 1 d . . .
H16C H 0.6362 0.2817 0.7990 0.069 Uiso 1 calc R . .
H16B H 0.7696 0.4651 0.8032 0.069 Uiso 1 calc R . .
H16A H 0.7288 0.3637 0.7348 0.069 Uiso 1 calc R . .
C17 C 0.2119(6) 0.7382(6) 0.6093(2) 0.0390(10) Uani 1 d . . .
H17C H 0.0867 0.6890 0.6000 0.059 Uiso 1 calc R . .
H17B H 0.2656 0.7803 0.5685 0.059 Uiso 1 calc R . .
H17A H 0.2485 0.8241 0.6432 0.059 Uiso 1 calc R . .
C18 C 0.1018(5) 0.4801(5) 0.6937(2) 0.0358(9) Uani 1 d . . .
H18C H -0.0068 0.4700 0.6718 0.054 Uiso 1 calc R . .
H18B H 0.1270 0.5382 0.7366 0.054 Uiso 1 calc R . .
H18A H 0.0927 0.3750 0.7007 0.054 Uiso 1 calc R . .
C19 C 0.2039(6) 0.4501(6) 0.5663(2) 0.0419(11) Uani 1 d . . .
H19C H 0.0816 0.4166 0.5539 0.063 Uiso 1 calc R . .
H19B H 0.2214 0.3578 0.5766 0.063 Uiso 1 calc R . .
H19A H 0.2696 0.5027 0.5291 0.063 Uiso 1 calc R . .
C20 C 0.8417(14) 1.4473(13) 1.0159(5) 0.114(3) Uiso 1 d D . .
C21 C 0.8804(12) 1.5138(11) 0.9563(4) 0.092(2) Uiso 1 d D . .
H21 H 0.7936 1.5205 0.9272 0.110 Uiso 1 calc R . .
C22 C 1.0322(12) 1.5669(12) 0.9393(5) 0.101(3) Uiso 1 d D . .
H22 H 1.0608 1.6147 0.8981 0.122 Uiso 1 calc R . .
C23 C 0.6831(19) 1.391(2) 1.0346(8) 0.083(4) Uiso 0.50 d PD . .
H23D H 0.6798 1.3470 1.0785 0.125 Uiso 0.50 calc PR . .
H23A H 0.6029 1.3079 1.0023 0.125 Uiso 0.50 calc PR . .
H23B H 0.6501 1.4761 1.0367 0.125 Uiso 0.50 calc PR . .
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'
P P 0.1023 0.0942 '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
N W P3 91.09(10) . . ?
N W Cl1 177.45(10) . . ?
P3 W Cl1 86.45(3) . . ?
N W P1 98.03(10) . . ?
P3 W P1 92.57(3) . . ?
Cl1 W P1 82.75(3) . . ?
N W P2 98.16(10) . . ?
P3 W P2 92.33(3) . . ?
Cl1 W P2 81.31(3) . . ?
P1 W P2 162.99(3) . . ?
N W Cl2 98.85(10) . . ?
P3 W Cl2 170.07(3) . . ?
Cl1 W Cl2 83.62(3) . . ?
P1 W Cl2 86.20(3) . . ?
P2 W Cl2 86.17(3) . . ?
C12 P1 C13 103.4(2) . . ?
C12 P1 C11 99.8(2) . . ?
C13 P1 C11 102.7(3) . . ?
C12 P1 W 118.95(15) . . ?
C13 P1 W 113.57(17) . . ?
C11 P1 W 116.16(17) . . ?
C15 P2 C14 103.2(2) . . ?
C15 P2 C16 102.8(2) . . ?
C14 P2 C16 100.2(2) . . ?
C15 P2 W 113.97(15) . . ?
C14 P2 W 118.03(16) . . ?
C16 P2 W 116.40(17) . . ?
C19 P3 C17 100.0(2) . . ?
C19 P3 C18 100.1(2) . . ?
C17 P3 C18 99.4(2) . . ?
C19 P3 W 116.93(15) . . ?
C17 P3 W 118.75(16) . . ?
C18 P3 W 118.10(15) . . ?
C1 N W 172.9(3) . . ?
N C1 C2 115.9(3) . . ?
N C1 C6 124.8(3) . . ?
C2 C1 C6 119.3(3) . . ?
C3 C2 C1 121.8(4) . . ?
C4 C3 C2 119.3(4) . . ?
C3 C4 C5 119.6(3) . . ?
C4 C5 C6 123.7(4) . . ?
C5 C6 C1 116.3(3) . . ?
C5 C6 C7 120.3(3) . . ?
C1 C6 C7 123.5(3) . . ?
C6 C7 C9 109.3(3) . . ?
C6 C7 C10 112.5(3) . . ?
C9 C7 C10 107.3(3) . . ?
C6 C7 C8 109.5(3) . . ?
C9 C7 C8 111.7(3) . . ?
C10 C7 C8 106.5(3) . . ?
C23 C20 C21 121.2(12) . . ?
C23 C20 C22 117.2(12) . 2_787 ?
C21 C20 C22 121.6(10) . 2_787 ?
C22 C21 C20 120.3(10) . . ?
C21 C22 C20 118.1(10) . 2_787 ?
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
W N 1.770(3) . ?
W P3 2.4845(10) . ?
W Cl1 2.4974(9) . ?
W P1 2.5039(10) . ?
W P2 2.5074(10) . ?
W Cl2 2.5096(9) . ?
P1 C12 1.824(4) . ?
P1 C13 1.825(5) . ?
P1 C11 1.831(5) . ?
P2 C15 1.826(4) . ?
P2 C14 1.828(5) . ?
P2 C16 1.833(5) . ?
P3 C19 1.832(4) . ?
P3 C17 1.840(4) . ?
P3 C18 1.844(4) . ?
N C1 1.409(4) . ?
C1 C2 1.410(5) . ?
C1 C6 1.435(5) . ?
C2 C3 1.389(5) . ?
C3 C4 1.384(6) . ?
C4 C5 1.384(6) . ?
C5 C6 1.403(5) . ?
C6 C7 1.528(5) . ?
C7 C9 1.542(5) . ?
C7 C10 1.546(5) . ?
C7 C8 1.551(5) . ?
C20 C23 1.321(14) . ?
C20 C21 1.347(11) . ?
C20 C22 1.412(10) 2_787 ?
C21 C22 1.257(10) . ?
C22 C20 1.412(10) 2_787 ?
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
N W P1 C11 107.7(2) . . . . ?
N W P1 C12 -133.1(2) . . . . ?
N W P1 C13 -11.1(2) . . . . ?
N W P2 C14 131.0(2) . . . . ?
N W P2 C15 9.6(2) . . . . ?
N W P2 C16 -109.9(2) . . . . ?
N W P3 C17 61.5(2) . . . . ?
N W P3 C18 -58.76(19) . . . . ?
N W P3 C19 -178.4(2) . . . . ?
