#------------------------------------------------------------------------------
#$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $
#$Revision: 14 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/1100715.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_1100715
_publ_requested_journal          'Inorganic Chemistry'
loop_
_publ_author_name
'Kay H. Horn'
'Natascha Bores'
'Nicolai Lehnert'
'Klaus Mersmann'
'Christian Nather'
'Gerhard Peters'
'Felix Tuczek'
_publ_section_title
;
Reduction Pathway of End-On Terminally Coordinated
Dinitrogen.  IV. Geometric, Electronic and Vibrational Structure of
a W(IV) Dialkylhydrazido Complex and its Two-Electron Reduced
Derivative Undergoing N-N Cleavage Upon Protonation
;
_chemical_formula_sum            'C57 H58 N2 P4 W'
_chemical_formula_weight         1078.79
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   12.6448(11)
_cell_length_b                   12.9364(12)
_cell_length_c                   16.7806(16)
_cell_angle_alpha                84.980(11)
_cell_angle_beta                 76.410(10)
_cell_angle_gamma                67.177(10)
_cell_volume                     2459.2(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    180(2)
_cell_measurement_reflns_used    7998
_cell_measurement_theta_min      11.5
_cell_measurement_theta_max      20.5
_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    2.519
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_diffrn_ambient_temperature      180(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       Phi-Scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16042
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.0830
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         24.94
_reflns_number_total             8020
_reflns_number_gt                6467
_reflns_threshold_expression     >2sigma(I)
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0027(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         8020
_refine_ls_number_parameters     621
_refine_ls_number_restraints     118
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.0989
_refine_ls_wR_factor_gt          0.0922
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
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 0.61866(2) 0.26517(2) 0.244537(14) 0.02035(10) Uani 1 1 d . . .
P1 P 0.70341(14) 0.35100(14) 0.32248(9) 0.0220(3) Uani 1 1 d . . .
P2 P 0.45459(14) 0.43240(14) 0.29642(8) 0.0210(3) Uani 1 1 d . . .
C1 C 0.5893(6) 0.4337(6) 0.4077(3) 0.0256(14) Uani 1 1 d . . .
H1A H 0.5641 0.3839 0.4492 0.031 Uiso 1 1 calc R . .
H1B H 0.6195 0.4787 0.4343 0.031 Uiso 1 1 calc R . .
C2 C 0.4859(6) 0.5110(6) 0.3701(3) 0.0247(13) Uani 1 1 d . . .
H2A H 0.5051 0.5737 0.3413 0.030 Uiso 1 1 calc R . .
H2B H 0.4150 0.5430 0.4144 0.030 Uiso 1 1 calc R . .
C11 C 0.8283(6) 0.2713(6) 0.3707(4) 0.0307(15) Uani 1 1 d . . .
C12 C 0.9226(7) 0.1856(7) 0.3258(5) 0.0419(18) Uani 1 1 d . . .
H12 H 0.9227 0.1702 0.2714 0.050 Uiso 1 1 calc R . .
C13 C 1.0172(9) 0.1224(9) 0.3607(7) 0.066(3) Uani 1 1 d . . .
H13 H 1.0815 0.0636 0.3296 0.079 Uiso 1 1 calc R . .
C14 C 1.0202(9) 0.1423(8) 0.4385(6) 0.057(2) Uani 1 1 d . . .
H14 H 1.0858 0.0984 0.4613 0.068 Uiso 1 1 calc R . .
C15 C 0.9275(8) 0.2264(9) 0.4826(5) 0.052(2) Uani 1 1 d . . .
H15 H 0.9285 0.2400 0.5371 0.063 Uiso 1 1 calc R . .
C16 C 0.8305(7) 0.2934(7) 0.4501(4) 0.0404(18) Uani 1 1 d . . .
H16 H 0.7674 0.3528 0.4814 0.048 Uiso 1 1 calc R . .
C21 C 0.7516(6) 0.4638(6) 0.2722(4) 0.0253(14) Uani 1 1 d . . .
C22 C 0.7090(7) 0.5168(7) 0.2046(4) 0.0404(19) Uani 1 1 d . . .
H22 H 0.6662 0.4878 0.1797 0.048 Uiso 1 1 calc R . .
C23 C 0.7286(8) 0.6123(7) 0.1730(4) 0.045(2) Uani 1 1 d . . .
H23 H 0.6971 0.6496 0.1275 0.055 Uiso 1 1 calc R . .
C24 C 0.7927(9) 0.6526(8) 0.2068(5) 0.054(2) Uani 1 1 d . . .
H24 H 0.8061 0.7177 0.1848 0.065 Uiso 1 1 calc R . .
C25 C 0.8384(9) 0.5993(9) 0.2732(5) 0.056(3) Uani 1 1 d . . .
H25 H 0.8841 0.6271 0.2962 0.068 Uiso 1 1 calc R . .
C26 C 0.8177(7) 0.5062(7) 0.3060(5) 0.0393(18) Uani 1 1 d . . .
H26 H 0.8485 0.4702 0.3520 0.047 Uiso 1 1 calc R . .
C31 C 0.3076(6) 0.4373(6) 0.3508(4) 0.0283(14) Uani 1 1 d . . .
C32 C 0.2905(7) 0.4103(6) 0.4338(4) 0.0365(17) Uani 1 1 d . . .
H32 H 0.3507 0.3992 0.4623 0.044 Uiso 1 1 calc R . .
C33 C 0.1860(9) 0.3992(9) 0.4755(5) 0.059(3) Uani 1 1 d . . .
H33 H 0.1739 0.3839 0.5327 0.070 Uiso 1 1 calc R . .
C34 C 0.1016(9) 0.4102(10) 0.4341(6) 0.070(3) Uani 1 1 d . . .
H34 H 0.0321 0.3990 0.4617 0.084 Uiso 1 1 calc R . .
C35 C 0.1172(8) 0.4379(9) 0.3517(6) 0.061(3) Uani 1 1 d . . .
H35 H 0.0577 0.4464 0.3233 0.073 Uiso 1 1 calc R . .
C36 C 0.2185(7) 0.4534(7) 0.3102(4) 0.0404(18) Uani 1 1 d . . .
H36 H 0.2270 0.4750 0.2542 0.049 Uiso 1 1 calc R . .
C41 C 0.4072(6) 0.5491(6) 0.2237(4) 0.0268(14) Uani 1 1 d . . .
C42 C 0.3274(7) 0.6553(6) 0.2501(5) 0.0381(17) Uani 1 1 d . . .
H42 H 0.2902 0.6674 0.3065 0.046 Uiso 1 1 calc R . .
C43 C 0.3009(9) 0.7434(7) 0.1961(5) 0.052(2) Uani 1 1 d . . .
H43 H 0.2470 0.8160 0.2154 0.062 Uiso 1 1 calc R . .
C44 C 0.3537(10) 0.7253(8) 0.1135(6) 0.061(3) Uani 1 1 d . . .
H44 H 0.3358 0.7858 0.0760 0.074 Uiso 1 1 calc R . .
C45 C 0.4318(9) 0.6203(8) 0.0854(5) 0.052(2) Uani 1 1 d . . .
H45 H 0.4664 0.6078 0.0286 0.062 Uiso 1 1 calc R . .
C46 C 0.4594(7) 0.5337(7) 0.1404(4) 0.0345(16) Uani 1 1 d . . .
H46 H 0.5151 0.4618 0.1211 0.041 Uiso 1 1 calc R . .
P3 P 0.63055(16) 0.12390(14) 0.35025(9) 0.0257(4) Uani 1 1 d . . .
P4 P 0.48201(15) 0.18338(15) 0.22039(9) 0.0242(4) Uani 1 1 d . . .
C3 C 0.5268(7) 0.0512(6) 0.3531(4) 0.0347(17) Uani 1 1 d . . .
H3A H 0.5691 -0.0202 0.3220 0.042 Uiso 1 1 calc R . .
H3B H 0.4973 0.0335 0.4105 0.042 Uiso 1 1 calc R . .
C4 C 0.4231(6) 0.1255(6) 0.3158(4) 0.0308(15) Uani 1 1 d . . .
H4A H 0.3681 0.1868 0.3542 0.037 Uiso 1 1 calc R . .
H4B H 0.3800 0.0807 0.3046 0.037 Uiso 1 1 calc R . .
C51 C 0.6092(7) 0.1453(6) 0.4616(4) 0.0332(16) Uani 1 1 d . . .
C52 C 0.7019(8) 0.1236(6) 0.5010(4) 0.0388(18) Uani 1 1 d . . .
H52 H 0.7810 0.0938 0.4708 0.047 Uiso 1 1 calc R . .
C53 C 0.6777(9) 0.1458(7) 0.5845(4) 0.044(2) Uani 1 1 d . . .
H53 H 0.7413 0.1286 0.6109 0.053 Uiso 1 1 calc R . .
C54 C 0.5652(9) 0.1915(7) 0.6295(4) 0.046(2) Uani 1 1 d . . .
H54 H 0.5507 0.2075 0.6861 0.055 Uiso 1 1 calc R . .
C55 C 0.4715(8) 0.2147(7) 0.5912(4) 0.0432(19) Uani 1 1 d . . .
H55 H 0.3928 0.2457 0.6217 0.052 Uiso 1 1 calc R . .
C56 C 0.4943(7) 0.1921(6) 0.5087(4) 0.0357(16) Uani 1 1 d . . .
H56 H 0.4302 0.2089 0.4830 0.043 Uiso 1 1 calc R . .
C61 C 0.7668(7) -0.0019(6) 0.3346(4) 0.0298(15) Uani 1 1 d . . .
C62 C 0.8533(8) -0.0156(7) 0.2626(4) 0.0402(18) Uani 1 1 d . . .
H62 H 0.8414 0.0426 0.2231 0.048 Uiso 1 1 calc R . .
C63 C 0.9543(8) -0.1093(7) 0.2469(5) 0.046(2) Uani 1 1 d . . .
H63 H 1.0115 -0.1148 0.1975 0.055 Uiso 1 1 calc R . .
C64 C 0.9734(8) -0.1961(7) 0.3027(5) 0.0422(19) Uani 1 1 d . . .
H64 H 1.0435 -0.2614 0.2920 0.051 Uiso 1 1 calc R . .
C65 C 0.8898(8) -0.1870(6) 0.3739(5) 0.0406(19) Uani 1 1 d . . .
H65 H 0.9025 -0.2466 0.4124 0.049 Uiso 1 1 calc R . .
C66 C 0.7881(7) -0.0926(6) 0.3902(4) 0.0328(16) Uani 1 1 d . . .
H66 H 0.7312 -0.0884 0.4395 0.039 Uiso 1 1 calc R . .
C71 C 0.3528(6) 0.2568(6) 0.1753(4) 0.0294(15) Uani 1 1 d . . .
C72 C 0.2439(7) 0.2437(8) 0.2052(5) 0.0433(19) Uani 1 1 d . . .
H72 H 0.2338 0.1966 0.2506 0.052 Uiso 1 1 calc R . .
C73 C 0.1518(8) 0.3027(8) 0.1657(6) 0.052(2) Uani 1 1 d . . .
H73 H 0.0776 0.2970 0.1864 0.062 Uiso 1 1 calc R . .
C74 C 0.1642(8) 0.3670(7) 0.0997(6) 0.051(2) Uani 1 1 d . . .
H74 H 0.1008 0.4032 0.0730 0.061 Uiso 1 1 calc R . .
C75 C 0.2708(8) 0.3803(7) 0.0705(5) 0.047(2) Uani 1 1 d . . .
H75 H 0.2799 0.4278 0.0251 0.056 Uiso 1 1 calc R . .
C76 C 0.3639(7) 0.3231(6) 0.1088(4) 0.0330(16) Uani 1 1 d . . .
H76 H 0.4372 0.3306 0.0878 0.040 Uiso 1 1 calc R . .
C81 C 0.5501(6) 0.0635(6) 0.1486(4) 0.0305(15) Uani 1 1 d . . .
C82 C 0.5094(8) -0.0229(7) 0.1544(5) 0.045(2) Uani 1 1 d . . .
H82 H 0.4494 -0.0256 0.1999 0.054 Uiso 1 1 calc R . .
C83 C 0.5552(10) -0.1044(8) 0.0950(6) 0.060(3) Uani 1 1 d . . .
H83 H 0.5279 -0.1641 0.1007 0.072 Uiso 1 1 calc R . .
C84 C 0.6398(9) -0.1014(7) 0.0273(6) 0.054(2) Uani 1 1 d . . .
H84 H 0.6693 -0.1572 -0.0141 0.065 Uiso 1 1 calc R . .
C85 C 0.6819(8) -0.0152(8) 0.0203(5) 0.051(2) Uani 1 1 d . . .
H85 H 0.7401 -0.0118 -0.0262 0.061 Uiso 1 1 calc R . .
C86 C 0.6383(7) 0.0651(7) 0.0814(4) 0.0406(19) Uani 1 1 d . . .
H86 H 0.6691 0.1222 0.0775 0.049 Uiso 1 1 calc R . .
N1 N 0.8015(5) 0.2355(5) 0.0745(3) 0.0305(13) Uani 1 1 d D . .
C91 C 0.9087(10) 0.1360(12) 0.0719(7) 0.036(3) Uani 0.574(17) 1 d PDU A 1
H91A H 0.8878 0.0699 0.0891 0.043 Uiso 0.574(17) 1 calc PR A 1
H91B H 0.9520 0.1454 0.1110 0.043 Uiso 0.574(17) 1 calc PR A 1
C92 C 0.9865(14) 0.1158(16) -0.0123(8) 0.053(4) Uani 0.574(17) 1 d PDU A 1
H92A H 1.0601 0.0502 -0.0109 0.064 Uiso 0.574(17) 1 calc PR A 1
H92B H 0.9465 0.0981 -0.0502 0.064 Uiso 0.574(17) 1 calc PR A 1
C93 C 1.0160(14) 0.2149(16) -0.0437(11) 0.050(4) Uani 0.574(17) 1 d PDU A 1
H93A H 1.0672 0.1993 -0.0994 0.060 Uiso 0.574(17) 1 calc PR A 1
H93B H 1.0578 0.2328 -0.0072 0.060 Uiso 0.574(17) 1 calc PR A 1
C94 C 0.899(2) 0.3139(19) -0.0459(9) 0.048(5) Uani 0.574(17) 1 d PDU A 1
H94A H 0.9146 0.3821 -0.0656 0.057 Uiso 0.574(17) 1 calc PR A 1
H94B H 0.8594 0.2966 -0.0844 0.057 Uiso 0.574(17) 1 calc PR A 1
C95 C 0.8213(14) 0.3342(13) 0.0377(8) 0.039(4) Uani 0.574(17) 1 d PDU A 1
H95A H 0.8570 0.3614 0.0737 0.047 Uiso 0.574(17) 1 calc PR A 1
H95B H 0.7445 0.3942 0.0346 0.047 Uiso 0.574(17) 1 calc PR A 1
C91' C 0.9216(13) 0.202(2) 0.0911(11) 0.054(6) Uani 0.426(17) 1 d PDU A 2
H91C H 0.9389 0.1340 0.1260 0.065 Uiso 0.426(17) 1 calc PR A 2
H91D H 0.9255 0.2628 0.1205 0.065 Uiso 0.426(17) 1 calc PR A 2
C92' C 1.010(2) 0.178(3) 0.0110(14) 0.078(8) Uani 0.426(17) 1 d PDU A 2
H92C H 1.0104 0.1122 -0.0155 0.093 Uiso 0.426(17) 1 calc PR A 2
H92D H 1.0892 0.1592 0.0212 0.093 Uiso 0.426(17) 1 calc PR A 2
C93' C 0.981(2) 0.280(2) -0.0474(13) 0.056(6) Uani 0.426(17) 1 d PDU A 2
H93C H 0.9959 0.3413 -0.0265 0.067 Uiso 0.426(17) 1 calc PR A 2
H93D H 1.0326 0.2583 -0.1026 0.067 Uiso 0.426(17) 1 calc PR A 2
C94' C 0.857(2) 0.319(3) -0.0529(11) 0.055(8) Uani 0.426(17) 1 d PDU A 2
H94C H 0.8461 0.2627 -0.0825 0.066 Uiso 0.426(17) 1 calc PR A 2
H94D H 0.8371 0.3897 -0.0850 0.066 Uiso 0.426(17) 1 calc PR A 2
C95' C 0.7750(5) 0.3402(4) 0.0293(3) 0.046(7) Uani 0.426(17) 1 d PDU A 2
H95C H 0.7847 0.3972 0.0596 0.055 Uiso 0.426(17) 1 calc PR A 2
H95D H 0.6927 0.3687 0.0229 0.055 Uiso 0.426(17) 1 calc PR A 2
N2 N 0.7195(5) 0.2498(4) 0.1482(3) 0.0253(12) Uani 1 1 d R A .