#------------------------------------------------------------------------------
#$Date: 2017-09-14 05:44:07 +0300 (Thu, 14 Sep 2017) $
#$Revision: 200875 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/42/7044223.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_7044223
loop_
_publ_author_name
'Schmid, Paul'
'Maier, Matthias'
'Pfeiffer, Hendrik'
'Belz, Anja'
'Henry, Lucas'
'Friedrich, Alexandra'
'Schönfeld, Fabian'
'Edkins, Katharina'
'Schatzschneider, Ulrich'
_publ_section_title
;
 Catalyst-free room-temperature iClick reaction of molybdenum(II) and
 tungsten(II) azide complexes with electron-poor alkynes: Structural
 preferences and kinetic studies
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03096G
_journal_year                    2017
_chemical_formula_moiety         'C15 H13 N5 O2 W'
_chemical_formula_sum            'C15 H13 N5 O2 W'
_chemical_formula_weight         479.15
_chemical_name_common            '[W(allyl)(N3)(bpy)(CO)2]'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-07-08
_audit_update_record
;
2017-07-17 deposited with the CCDC.
2017-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.83(3)
_cell_length_b                   13.769(17)
_cell_length_c                   6.602(8)
_cell_measurement_reflns_used    3245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.47
_cell_measurement_theta_min      2.42
_cell_volume                     1530(4)
_computing_cell_refinement       'Saint+ ver. V8.34A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 2014.11-0 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. V8.34A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD area detector (Apex2)'
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9425
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.279
_diffrn_reflns_theta_min         2.837
_diffrn_source                   'rotating-anode (Nonius FR-591)'
_exptl_absorpt_coefficient_mu    7.566
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs 2014/5 (Bruker AXS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_description       plate
_exptl_crystal_F_000             912
_exptl_crystal_preparation
'Crystal fragment soaked in perfluoro polyether oil.'
_exptl_crystal_recrystallization_method
'recrystallised from acetone and methanol by evaporation'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.321
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         1979
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0109P)²+1.3487P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1427
_reflns_number_total             1979
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03096g2.cif
_cod_data_source_block           af051_final
_cod_database_code               7044223
_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.
;
_shelx_estimated_absorpt_t_min   0.161
_shelx_estimated_absorpt_t_max   0.583
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
W1 W 0.49947(2) 0.2500 0.32134(2) 0.01032(6) Uani 1 2 d S T P
C1 C 0.5773(2) 0.1565(2) 0.4248(5) 0.0165(7) Uani 1 1 d . . .
N1 N 0.5558(3) 0.2500 0.0260(6) 0.0154(8) Uani 1 2 d S T P
O1 O 0.62320(17) 0.10061(18) 0.4852(4) 0.0257(6) Uani 1 1 d . . .
C3 C 0.3701(2) -0.0019(2) 0.0433(5) 0.0206(8) Uani 1 1 d . . .
H3 H 0.3761 -0.0705 0.0436 0.025 Uiso 1 1 calc R U .
N3 N 0.6935(3) 0.2500 -0.0399(8) 0.0303(11) Uani 1 2 d S T P
N4 N 0.41598(17) 0.15437(19) 0.1520(4) 0.0108(6) Uani 1 1 d . . .
C4 C 0.3093(2) 0.0413(3) -0.0622(5) 0.0211(8) Uani 1 1 d . . .
H4 H 0.2722 0.0027 -0.1347 0.025 Uiso 1 1 calc R U .
N2 N 0.6263(3) 0.2500 -0.0005(6) 0.0175(9) Uani 1 2 d S T P
C2 C 0.4222(2) 0.0567(2) 0.1489(5) 0.0158(7) Uani 1 1 d . . .
H2 H 0.4642 0.0270 0.2225 0.019 Uiso 1 1 calc R U .
C7 C 0.4477(2) 0.1637(3) 0.5923(5) 0.0193(8) Uani 1 1 d . . .
H7A H 0.487(2) 0.160(3) 0.707(6) 0.023 Uiso 1 1 d . U .
H7B H 0.426(3) 0.105(3) 0.557(6) 0.023 Uiso 1 1 d . U .
C6 C 0.3571(2) 0.1961(2) 0.0437(5) 0.0111(6) Uani 1 1 d . . .
C8 C 0.4050(3) 0.2500 0.5527(7) 0.0181(10) Uani 1 2 d S T P
H8 H 0.358(4) 0.2500 0.502(8) 0.022 Uiso 1 2 d S U P
C5 C 0.3026(2) 0.1412(2) -0.0623(5) 0.0168(7) Uani 1 1 d . . .
H5 H 0.2608 0.1719 -0.1346 0.020 Uiso 1 1 calc R U .
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1.00 0.00 0.00 0.0530
-1.00 -2.00 -1.00 0.0830
1.00 2.00 1.00 0.1640
0.00 2.00 1.00 0.1220
-1.00 2.00 1.00 0.0920
-2.00 1.00 0.00 0.0600
2.00 -2.00 -1.00 0.2000
1.00 2.00 2.00 0.1480
-2.00 2.00 1.00 0.0750
0.00 -1.00 -1.00 0.1360
0.00 1.00 1.00 0.0930
-2.00 -1.00 -2.00 0.0720
2.00 1.00 2.00 0.1450
1.00 -2.00 -2.00 0.1790
0.00 1.00 2.00 0.0660
1.00 1.00 3.00 0.1180
0.00 0.00 1.00 0.0200
0.00 -3.00 -1.00 0.1500
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
C1 W1 C1 82.2(2) . 8_565
C1 W1 N1 91.20(15) . .
C1 W1 N1 91.20(15) 8_565 .
C1 W1 C8 103.92(17) . .
C1 W1 C8 103.92(17) 8_565 .
N1 W1 C8 159.79(18) . .
C1 W1 N4 102.02(15) . .
C1 W1 N4 170.17(11) 8_565 .
N1 W1 N4 79.90(14) . .
C8 W1 N4 83.84(16) . .
C1 W1 N4 170.17(11) . 8_565
C1 W1 N4 102.02(15) 8_565 8_565
N1 W1 N4 79.90(14) . 8_565
C8 W1 N4 83.84(16) . 8_565
N4 W1 N4 72.49(17) . 8_565
C1 W1 C7 69.22(16) . .
C1 W1 C7 108.62(15) 8_565 .
N1 W1 C7 149.15(10) . .
C8 W1 C7 36.32(13) . .
N4 W1 C7 81.21(14) . .
N4 W1 C7 116.97(15) 8_565 .
C1 W1 C7 108.62(15) . 8_565
C1 W1 C7 69.22(16) 8_565 8_565
N1 W1 C7 149.15(10) . 8_565
C8 W1 C7 36.32(13) . 8_565
N4 W1 C7 116.97(15) . 8_565
N4 W1 C7 81.21(14) 8_565 8_565
C7 W1 C7 61.7(2) . 8_565
O1 C1 W1 179.6(3) . .
N2 N1 W1 124.3(3) . .
C4 C3 C2 118.5(3) . .
C4 C3 H3 120.8 . .
C2 C3 H3 120.8 . .
C2 N4 C6 118.3(3) . .
C2 N4 W1 123.2(2) . .
C6 N4 W1 118.5(2) . .
C3 C4 C5 119.5(3) . .
C3 C4 H4 120.2 . .
C5 C4 H4 120.2 . .
N3 N2 N1 175.4(5) . .
N4 C2 C3 122.7(3) . .
N4 C2 H2 118.6 . .
C3 C2 H2 118.6 . .
C8 C7 W1 67.5(2) . .
C8 C7 H7A 121(3) . .
W1 C7 H7A 111(2) . .
C8 C7 H7B 120(3) . .
W1 C7 H7B 114(2) . .
H7A C7 H7B 114(4) . .
N4 C6 C5 121.6(3) . .
N4 C6 C6 115.19(18) . 8_565
C5 C6 C6 123.23(19) . 8_565
C7 C8 C7 114.5(5) . 8_565
C7 C8 W1 76.2(3) . .
C7 C8 W1 76.2(3) 8_565 .
C7 C8 H8 122.7(3) . .
C7 C8 H8 122.7(3) 8_565 .
W1 C8 H8 113(4) . .
C6 C5 C4 119.4(3) . .
C6 C5 H5 120.3 . .
C4 C5 H5 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 C1 1.959(4) .
W1 C1 1.960(4) 8_565
W1 N1 2.169(5) .
W1 C8 2.205(5) .
W1 N4 2.227(3) .
W1 N4 2.227(3) 8_565
W1 C7 2.318(4) .
W1 C7 2.318(4) 8_565
C1 O1 1.161(4) .
N1 N2 1.199(6) .
C3 C4 1.372(6) .
C3 C2 1.381(5) .
C3 H3 0.9500 .
N3 N2 1.160(7) .
N4 C2 1.349(4) .
N4 C6 1.350(4) .
C4 C5 1.380(5) .
C4 H4 0.9500 .
C2 H2 0.9500 .
C7 C8 1.413(5) .
C7 H7A 1.01(4) .
C7 H7B 0.91(4) .
C6 C5 1.380(5) .
C6 C6 1.484(6) 8_565
C8 C7 1.413(5) 8_565
C8 H8 0.86(6) .
C5 H5 0.9500 .
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
C2 C3 C4 C5 0.9(5) . .
C6 N4 C2 C3 -1.3(5) . .
W1 N4 C2 C3 -180.0(3) . .
C4 C3 C2 N4 -0.2(5) . .
C2 N4 C6 C5 2.3(5) . .
W1 N4 C6 C5 -179.0(2) . .
C2 N4 C6 C6 -176.2(2) . 8_565
W1 N4 C6 C6 2.5(2) . 8_565
W1 C7 C8 C7 -67.6(4) . 8_565
N4 C6 C5 C4 -1.7(5) . .
C6 C6 C5 C4 176.7(2) 8_565 .
C3 C4 C5 C6 0.0(5) . .
