#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:31:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179505 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/02/4340287.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_4340287
loop_
_publ_author_name
'Rische, Daniel'
'Baunemann, Arne'
'Winter, Manuela'
'Fischer, Roland A.'
_publ_section_title
;
 Mixed guanidinato/alkylimido/azido tungsten(VI) complexes: synthesis and
 structural characterization.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              269
_journal_page_last               277
_journal_paper_doi               10.1021/ic0512431
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C26 H60 N16 W2'
_chemical_formula_weight         964.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.507(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3581(8)
_cell_length_b                   21.4148(18)
_cell_length_c                   10.0342(9)
_cell_measurement_reflns_used    3970
_cell_measurement_temperature    105(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      3.00
_cell_volume                     1883.4(3)
_computing_cell_refinement       'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_data_collection       'CrysAlis CCD 1.171.13, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 1.171.13, Oxford Diffraction'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  SHELXTL-PLUS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      105(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '560 images at 1.0 deg in ω and 15 sec'
_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  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            18548
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    6.143
_exptl_absorpt_correction_T_max  0.481
_exptl_absorpt_correction_T_min  0.156
_exptl_absorpt_correction_type   'numeric analytical'
_exptl_absorpt_process_details   'Gaussian face-indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.131
_refine_diff_density_min         -2.220
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0510
_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)+(0.0125P)²+37.3733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.0997
_reflns_number_gt                3842
_reflns_number_total             4295
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0512431si20050725_093124.cif
_cod_data_source_block           7
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4340287
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.91622(3) 0.064248(12) 0.40901(3) 0.01298(9) Uani 1 1 d .
C22 C 0.945(2) 0.0757(7) 0.0207(15) 0.085(5) Uani 1 1 d .
H1A H 1.0364 0.0492 0.0544 0.127 Uiso 1 1 calc R
H1B H 0.9398 0.0960 -0.0685 0.127 Uiso 1 1 calc R
H1C H 0.8542 0.0499 0.0043 0.127 Uiso 1 1 calc R
C23 C 1.0934(14) 0.1634(7) 0.1623(14) 0.070(4) Uani 1 1 d .
H2A H 1.0987 0.1952 0.2341 0.105 Uiso 1 1 calc R
H2B H 1.0916 0.1838 0.0742 0.105 Uiso 1 1 calc R
H2C H 1.1829 0.1361 0.1974 0.105 Uiso 1 1 calc R
C21 C 0.8130(13) 0.1637(8) 0.0750(14) 0.084(6) Uani 1 1 d .
H3A H 0.8125 0.1964 0.1431 0.125 Uiso 1 1 calc R
H3B H 0.7237 0.1367 0.0578 0.125 Uiso 1 1 calc R
H3C H 0.8095 0.1829 -0.0147 0.125 Uiso 1 1 calc R
C20 C 0.9538(9) 0.1260(4) 0.1338(8) 0.0227(16) Uani 1 1 d .
N2 N 0.9534(7) 0.0934(3) 0.2615(7) 0.0210(13) Uani 1 1 d .
N1 N 0.8960(7) 0.1270(3) 0.5140(7) 0.0179(12) Uani 1 1 d .
C10 C 0.8910(8) 0.1930(3) 0.5493(8) 0.0201(15) Uani 1 1 d .
C13 C 1.0423(11) 0.2200(6) 0.5558(12) 0.057(4) Uani 1 1 d .
H8A H 1.0528 0.2162 0.4623 0.086 Uiso 1 1 calc R
H8B H 1.1253 0.1972 0.6266 0.086 Uiso 1 1 calc R
H8C H 1.0471 0.2642 0.5827 0.086 Uiso 1 1 calc R
C11 C 0.7534(10) 0.2235(4) 0.4375(9) 0.0279(18) Uani 1 1 d .
H9A H 0.7630 0.2197 0.3436 0.042 Uiso 1 1 calc R
H9B H 0.7491 0.2677 0.4607 0.042 Uiso 1 1 calc R
H9C H 0.6598 0.2026 0.4363 0.042 Uiso 1 1 calc R
N3 N 1.1224(6) 0.0281(3) 0.5407(6) 0.0126(11) Uani 1 1 d .
C30 C 1.2523(7) 0.0607(3) 0.5883(7) 0.0154(13) Uani 1 1 d .
N6 N 0.6774(7) 0.0529(3) 0.2956(7) 0.0211(13) Uani 1 1 d .
N4 N 1.3043(7) 0.0854(3) 0.7209(7) 0.0215(13) Uani 1 1 d .
N7 N 0.5838(7) 0.0906(3) 0.2329(7) 0.0184(13) Uani 1 1 d .
N8 N 0.4858(7) 0.1233(3) 0.1700(8) 0.0289(16) Uani 1 1 d .
C34 C 1.4672(9) 0.0894(4) 0.8051(11) 0.036(2) Uani 1 1 d .
H13A H 1.5255 0.0931 0.7412 0.055 Uiso 1 1 calc R
H13B H 1.4989 0.0516 0.8632 0.055 Uiso 1 1 calc R
H13C H 1.4861 0.1261 0.8673 0.055 Uiso 1 1 calc R
C33 C 1.2111(10) 0.0795(4) 0.8061(9) 0.030(2) Uani 1 1 d .
H14A H 1.1037 0.0771 0.7443 0.045 Uiso 1 1 calc R
H14B H 1.2262 0.1159 0.8687 0.045 Uiso 1 1 calc R
H14C H 1.2393 0.0415 0.8638 0.045 Uiso 1 1 calc R
N5 N 1.3354(7) 0.0700(3) 0.5036(7) 0.0219(13) Uani 1 1 d .
C32 C 1.4267(9) 0.1263(4) 0.5087(11) 0.036(2) Uani 1 1 d .
H16A H 1.4346 0.1506 0.5937 0.053 Uiso 1 1 calc R
H16B H 1.3773 0.1516 0.4236 0.053 Uiso 1 1 calc R
H16C H 1.5289 0.1142 0.5122 0.053 Uiso 1 1 calc R
C31 C 1.3137(9) 0.0281(4) 0.3831(9) 0.0243(17) Uani 1 1 d .
H17A H 1.2523 -0.0078 0.3907 0.036 Uiso 1 1 calc R
H17B H 1.4132 0.0137 0.3836 0.036 Uiso 1 1 calc R
H17C H 1.2610 0.0505 0.2942 0.036 Uiso 1 1 calc R
C12 C 0.8749(10) 0.1989(4) 0.6955(9) 0.0272(18) Uani 1 1 d .
H18A H 0.9630 0.1795 0.7678 0.041 Uiso 1 1 calc R
H18B H 0.7812 0.1779 0.6939 0.041 Uiso 1 1 calc R
H18C H 0.8700 0.2432 0.7184 0.041 Uiso 1 1 calc R
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'
W W -0.8490 6.8722 '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'
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
N2 W1 N1 109.3(3) . .
N2 W1 N3 104.9(2) . .
N1 W1 N3 100.1(2) . .
N2 W1 N3 129.8(3) . 3_756
N1 W1 N3 120.7(3) . 3_756
N3 W1 N3 72.2(2) . 3_756
N2 W1 N6 94.1(3) . .
N1 W1 N6 95.4(3) . .
N3 W1 N6 149.8(2) . .
N3 W1 N6 77.6(2) 3_756 .
N2 C20 C23 111.4(7) . .
N2 C20 C21 109.5(7) . .
C23 C20 C21 112.7(10) . .
N2 C20 C22 107.2(8) . .
C23 C20 C22 109.6(10) . .
C21 C20 C22 106.1(11) . .
C20 N2 W1 167.2(5) . .
C10 N1 W1 154.6(5) . .
N1 C10 C13 105.8(7) . .
N1 C10 C11 109.0(6) . .
C13 C10 C11 113.9(8) . .
N1 C10 C12 109.5(6) . .
C13 C10 C12 109.4(7) . .
C11 C10 C12 109.1(6) . .
C30 N3 W1 124.1(5) . .
C30 N3 W1 128.1(5) . 3_756
W1 N3 W1 107.8(2) . 3_756
N3 C30 N5 120.2(6) . .
N3 C30 N4 121.7(6) . .
N5 C30 N4 118.1(6) . .
N7 N6 W1 129.8(5) . .
C30 N4 C33 118.0(6) . .
C30 N4 C34 122.2(7) . .
C33 N4 C34 113.0(7) . .
N8 N7 N6 174.9(8) . .
C30 N5 C31 119.0(6) . .
C30 N5 C32 123.7(7) . .
C31 N5 C32 116.3(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 N2 1.750(6) .
W1 N1 1.758(6) .
W1 N3 2.069(6) .
W1 N3 2.103(6) 3_756
W1 N6 2.137(6) .
C22 C20 1.547(15) .
C23 C20 1.473(13) .
C21 C20 1.481(13) .
C20 N2 1.460(9) .
N1 C10 1.462(9) .
C10 C13 1.510(10) .
C10 C11 1.527(10) .
C10 C12 1.532(11) .
N3 C30 1.337(9) .
N3 W1 2.103(6) 3_756
C30 N5 1.354(9) .
C30 N4 1.354(9) .
N6 N7 1.195(8) .
N4 C33 1.425(11) .
N4 C34 1.463(10) .
N7 N8 1.152(9) .
N5 C31 1.461(10) .
N5 C32 1.467(10) .
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_4
C23 C20 N2 W1 119(3) . .
C21 C20 N2 W1 -6(3) . .
C22 C20 N2 W1 -121(3) . .
N1 W1 N2 C20 -53(3) . .
N3 W1 N2 C20 -159(3) . .
N3 W1 N2 C20 122(3) 3_756 .
N6 W1 N2 C20 44(3) . .
N2 W1 N1 C10 1.1(13) . .
N3 W1 N1 C10 110.9(12) . .
N3 W1 N1 C10 -173.9(11) 3_756 .
N6 W1 N1 C10 -95.1(12) . .
W1 N1 C10 C13 -57.2(14) . .
W1 N1 C10 C11 65.6(14) . .
W1 N1 C10 C12 -175.1(10) . .
N2 W1 N3 C30 55.5(6) . .
N1 W1 N3 C30 -57.7(6) . .
N3 W1 N3 C30 -176.8(7) 3_756 .
N6 W1 N3 C30 -177.4(5) . .
N2 W1 N3 W1 -127.6(3) . 3_756
N1 W1 N3 W1 119.2(3) . 3_756
N3 W1 N3 W1 0.0 3_756 3_756
N6 W1 N3 W1 -0.5(6) . 3_756
W1 N3 C30 N5 -79.9(8) . .
W1 N3 C30 N5 103.9(7) 3_756 .
W1 N3 C30 N4 99.9(7) . .
W1 N3 C30 N4 -76.3(8) 3_756 .
N2 W1 N6 N7 -58.0(7) . .
N1 W1 N6 N7 51.8(7) . .
N3 W1 N6 N7 172.6(6) . .
N3 W1 N6 N7 172.1(8) 3_756 .
N3 C30 N4 C33 -4.3(11) . .
N5 C30 N4 C33 175.5(7) . .
N3 C30 N4 C34 144.9(8) . .
N5 C30 N4 C34 -35.3(11) . .
W1 N6 N7 N8 180(100) . .
N3 C30 N5 C31 -20.8(10) . .
N4 C30 N5 C31 159.5(7) . .
N3 C30 N5 C32 147.7(7) . .
N4 C30 N5 C32 -32.1(11) . .
