#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/11/78/4117881.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_4117881
loop_
_publ_author_name
'Ian A. Tonks'
'Alec C. Durrell'
'Harry B. Gray'
'John E. Bercaw'
_publ_contact_author
;       Michael W. Day
        Beckman Institute
        California Institute of Technology
        Pasadena, CA  91125
        USA
;
_publ_contact_author_email       mikeday@caltech.edu
_publ_contact_author_fax         '(818) 449 4159'
_publ_contact_author_phone       '(818) 395 2734'
_publ_section_title
;
 Groups 5 and 6 Terminal Hydrazido(2-) Complexes: Nβ Substituent Effects
 on Ligand-to-Metal Charge-Transfer Energies and Oxidation States
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7301
_journal_page_last               7304
_journal_paper_doi               10.1021/ja302275j
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C7 H13 Cl4 N3 W'
_chemical_formula_sum            'C7 H13 Cl4 N3 W'
_chemical_formula_weight         464.85
_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                 92.958(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6582(4)
_cell_length_b                   14.7762(7)
_cell_length_c                   9.7818(4)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      50.15
_cell_measurement_theta_min      2.50
_cell_volume                     1394.12(10)
_computing_cell_refinement       'Bruker SAINT-Plus v7.68A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.68A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       'ω scans; 20 settings'
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0218
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            146180
_diffrn_reflns_theta_full        53.16
_diffrn_reflns_theta_max         53.16
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    9.026
_exptl_absorpt_correction_T_max  0.6815
_exptl_absorpt_correction_T_min  0.2405
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2009/1, Bruker-AXS, Madison'
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    2.215
_exptl_crystal_description       'Triangular - Fragment'
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.633
_refine_diff_density_min         -2.258
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.462
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     137
_refine_ls_number_reflns         16520
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.462
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0210
_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/s²(Fo²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0323
_refine_ls_wR_factor_ref         0.0335
_reflns_number_gt                13350
_reflns_number_total             16520
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja302275j_si_002_01.cif
_cod_data_source_block           3i
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_database_code               4117881
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 0.797244(3) 0.322461(2) -0.023457(3) 0.01123(1) Uani 1 1 d .
Cl1 Cl 0.94276(2) 0.415921(17) -0.14956(2) 0.01974(4) Uani 1 1 d .
Cl2 Cl 0.98352(2) 0.228761(17) 0.03826(3) 0.02169(4) Uani 1 1 d .
Cl3 Cl 0.64313(2) 0.220462(18) 0.07617(3) 0.02281(4) Uani 1 1 d .
Cl4 Cl 0.60453(2) 0.391775(17) -0.13562(2) 0.01872(4) Uani 1 1 d .
N1 N 0.80672(7) 0.38987(5) 0.12423(7) 0.01295(10) Uani 1 1 d .
N2 N 0.81123(8) 0.43380(6) 0.23560(8) 0.01801(14) Uani 1 1 d .
N3 N 0.78491(9) 0.23278(6) -0.20726(9) 0.01895(14) Uani 1 1 d .
C1 C 0.90670(9) 0.40643(8) 0.35029(9) 0.02023(17) Uani 1 1 d .
H1A H 0.9760 0.4547 0.3699 0.024 Uiso 1 1 calc R
H1B H 0.9566 0.3506 0.3261 0.024 Uiso 1 1 calc R
C2 C 0.82385(10) 0.38958(8) 0.47592(10) 0.02015(16) Uani 1 1 d .
H2A H 0.7660 0.3348 0.4611 0.024 Uiso 1 1 calc R
H2B H 0.8884 0.3785 0.5561 0.024 Uiso 1 1 calc R
C3 C 0.73121(11) 0.46968(9) 0.50524(10) 0.02349(19) Uani 1 1 d .
H3A H 0.7894 0.5234 0.5278 0.028 Uiso 1 1 calc R
H3B H 0.6763 0.4559 0.5854 0.028 Uiso 1 1 calc R
C4 C 0.63313(10) 0.49087(8) 0.38156(10) 0.02069(17) Uani 1 1 d .
H4A H 0.5694 0.4392 0.3640 0.025 Uiso 1 1 calc R
H4B H 0.5767 0.5447 0.4015 0.025 Uiso 1 1 calc R
C5 C 0.71423(10) 0.50861(6) 0.25524(9) 0.01656(14) Uani 1 1 d .
H5A H 0.6495 0.5142 0.1738 0.020 Uiso 1 1 calc R
H5B H 0.7662 0.5661 0.2664 0.020 Uiso 1 1 calc R
C6 C 0.78490(10) 0.18772(7) -0.30180(11) 0.01906(15) Uani 1 1 d .
C7 C 0.78612(13) 0.13029(8) -0.42200(12) 0.0270(2) Uani 1 1 d .
H7A H 0.8718 0.1406 -0.4692 0.040 Uiso 1 1 calc R
H7B H 0.7061 0.1447 -0.4838 0.040 Uiso 1 1 calc R
H7C H 0.7814 0.0667 -0.3942 0.040 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
W1 0.01136(1) 0.01174(1) 0.01049(1) -0.00064(1) -0.00032(1) -0.00001(1)
Cl1 0.02119(9) 0.02264(10) 0.01590(8) 0.00019(7) 0.00583(7) -0.00531(7)
Cl2 0.01741(8) 0.01998(10) 0.02712(11) -0.00008(8) -0.00450(7) 0.00564(7)
Cl3 0.02096(9) 0.02017(10) 0.02737(11) 0.00556(8) 0.00196(8) -0.00663(7)
Cl4 0.01657(8) 0.02141(9) 0.01772(9) 0.00103(7) -0.00341(6) 0.00443(7)
N1 0.0130(2) 0.0158(3) 0.0101(2) 0.0005(2) 0.00129(19) -0.0003(2)
N2 0.0181(3) 0.0254(4) 0.0102(3) -0.0037(2) -0.0021(2) 0.0079(3)
N3 0.0192(3) 0.0188(3) 0.0186(3) -0.0049(3) -0.0017(3) 0.0007(3)
C1 0.0139(3) 0.0345(5) 0.0121(3) -0.0007(3) -0.0013(2) 0.0060(3)
C2 0.0179(3) 0.0272(5) 0.0153(3) 0.0059(3) 0.0004(3) 0.0037(3)
C3 0.0244(4) 0.0340(5) 0.0126(3) 0.0021(3) 0.0053(3) 0.0077(4)
C4 0.0185(3) 0.0264(5) 0.0176(4) 0.0048(3) 0.0056(3) 0.0078(3)
C5 0.0208(3) 0.0154(3) 0.0136(3) 0.0010(3) 0.0023(3) 0.0039(3)
C6 0.0205(3) 0.0168(4) 0.0197(4) -0.0041(3) -0.0009(3) 0.0017(3)
C7 0.0329(5) 0.0229(5) 0.0249(5) -0.0119(4) -0.0015(4) 0.0050(4)
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'
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
N1 W1 N3 178.19(3)
N1 W1 Cl2 96.75(2)
N3 W1 Cl2 82.19(2)
N1 W1 Cl4 98.26(2)
N3 W1 Cl4 82.78(2)
Cl2 W1 Cl4 164.964(9)
N1 W1 Cl1 95.22(2)
N3 W1 Cl1 86.27(2)
Cl2 W1 Cl1 90.597(10)
Cl4 W1 Cl1 88.833(9)
N1 W1 Cl3 91.70(2)
N3 W1 Cl3 86.85(2)
Cl2 W1 Cl3 90.491(10)
Cl4 W1 Cl3 88.275(9)
Cl1 W1 Cl3 172.817(9)
N2 N1 W1 176.04(7)
N1 N2 C5 120.29(7)
N1 N2 C1 120.47(8)
C5 N2 C1 119.09(8)
C6 N3 W1 176.86(8)
N2 C1 C2 109.01(7)
C3 C2 C1 111.37(9)
C2 C3 C4 110.89(9)
C5 C4 C3 110.75(8)
N2 C5 C4 109.61(8)
N3 C6 C7 179.53(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
W1 N1 1.7533(7)
W1 N3 2.2317(8)
W1 Cl2 2.3251(2)
W1 Cl4 2.3465(2)
W1 Cl1 2.3628(2)
W1 Cl3 2.3636(2)
N1 N2 1.2669(11)
N2 C5 1.4680(12)
N2 C1 1.4716(12)
N3 C6 1.1395(13)
C1 C2 1.5212(13)
C2 C3 1.5199(15)
C3 C4 1.5299(14)
C4 C5 1.5195(13)
C6 C7 1.4506(14)
