#------------------------------------------------------------------------------
#$Date: 2017-10-13 11:03:29 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201974 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/21/26/2212665.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2212665
loop_
_publ_author_name
'Wei Xu'
'Jian-Li Lin'
_publ_section_title
;
 Dichloridobis(1,10-phenanthroline-κ²N,N')tungsten(II)
;
_journal_coeditor_code           PK2005
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m859
_journal_page_last               m861
_journal_paper_doi               10.1107/S1600536807008148
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[W Cl2 (C12 H8 N2)2]'
_chemical_formula_moiety         'C24 H16 Cl2 N4 W'
_chemical_formula_sum            'C24 H16 Cl2 N4 W'
_chemical_formula_weight         615.15
_chemical_name_systematic
;
Dichloridobis(1,10-phenanthroline-κ²N,N')tungsten(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 100.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.6728(19)
_cell_length_b                   15.004(3)
_cell_length_c                   14.730(3)
_cell_measurement_reflns_used    16372
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     2105.0(8)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2004)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_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  0.0383
_diffrn_reflns_av_sigmaI/netI    0.0317
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20260
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.06
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.762
_exptl_absorpt_correction_T_max  0.270
_exptl_absorpt_correction_T_min  0.146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.762
_refine_diff_density_min         -0.456
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0247P)²+1.4626P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0570
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                3962
_reflns_number_total             4790
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2212665
_cod_database_fobs_code          2212665
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
W W 0.267980(16) 0.221072(10) 0.952477(10) 0.03748(6) Uani d . 1
Cl Cl1 0.46238(12) 0.20569(8) 1.08954(8) 0.0579(3) Uani d . 1
Cl Cl2 0.31822(12) 0.13161(8) 0.81942(8) 0.0575(3) Uani d . 1
N N1 0.3337(4) 0.3629(2) 0.8835(2) 0.0471(8) Uani d . 1
N N2 0.1768(4) 0.3578(2) 1.0227(2) 0.0452(8) Uani d . 1
N N3 0.0086(4) 0.2183(2) 0.8719(2) 0.0466(8) Uani d . 1
N N4 0.1093(3) 0.1357(2) 1.0353(2) 0.0381(7) Uani d . 1
C C1 0.4103(5) 0.3646(4) 0.8181(3) 0.0587(12) Uani d . 1
H H1 0.4246 0.3118 0.7879 0.070 Uiso calc R 1
C C2 0.4711(5) 0.4432(4) 0.7924(4) 0.0690(15) Uani d . 1
H H2 0.5244 0.4426 0.7456 0.083 Uiso calc R 1
C C3 0.4514(5) 0.5209(4) 0.8367(4) 0.0680(15) Uani d . 1
H H3 0.4928 0.5734 0.8212 0.082 Uiso calc R 1
C C4 0.3686(5) 0.5208(3) 0.9054(3) 0.0582(12) Uani d . 1
C C5 0.3410(6) 0.6005(3) 0.9529(4) 0.0718(16) Uani d . 1
H H5 0.3788 0.6545 0.9381 0.086 Uiso calc R 1
C C6 0.2603(6) 0.5975(3) 1.0193(4) 0.0713(16) Uani d . 1
H H6 0.2436 0.6500 1.0492 0.086 Uiso calc R 1
C C7 0.1997(5) 0.5160(3) 1.0452(3) 0.0539(12) Uani d . 1
C C8 0.1180(5) 0.5104(3) 1.1138(3) 0.0623(13) Uani d . 1
H H8 0.0994 0.5615 1.1452 0.075 Uiso calc R 1
C C9 0.0654(6) 0.4309(3) 1.1351(3) 0.0633(13) Uani d . 1
H H9 0.0088 0.4266 1.1799 0.076 Uiso calc R 1
C C10 0.0990(5) 0.3555(3) 1.0877(3) 0.0557(11) Uani d . 1
H H10 0.0644 0.3006 1.1029 0.067 Uiso calc R 1
C C11 0.2285(4) 0.4375(2) 1.0004(3) 0.0427(9) Uani d . 1
C C12 0.3120(4) 0.4396(3) 0.9273(3) 0.0439(9) Uani d . 1
C C13 -0.0397(6) 0.2567(3) 0.7913(3) 0.0606(13) Uani d . 1
H H13 0.0230 0.2871 0.7613 0.073 Uiso calc R 1
C C14 -0.1804(7) 0.2532(3) 0.7501(4) 0.0714(16) Uani d . 1
H H14 -0.2108 0.2808 0.6937 0.086 Uiso calc R 1
C C15 -0.2729(6) 0.2088(3) 0.7935(4) 0.0662(15) Uani d . 1
H H15 -0.3673 0.2060 0.7667 0.079 Uiso calc R 1
C C16 -0.2259(4) 0.1672(3) 0.8784(3) 0.0513(11) Uani d . 1
C C17 -0.3163(5) 0.1183(4) 0.9275(4) 0.0675(14) Uani d . 1
H H17 -0.4117 0.1148 0.9033 0.081 Uiso calc R 1
C C18 -0.2668(5) 0.0774(3) 1.0075(4) 0.0632(13) Uani d . 1
H H18 -0.3283 0.0462 1.0378 0.076 Uiso calc R 1
C C19 -0.1205(4) 0.0810(3) 1.0469(3) 0.0467(10) Uani d . 1
C C20 -0.0641(5) 0.0387(3) 1.1297(3) 0.0538(11) Uani d . 1
H H20 -0.1220 0.0062 1.1617 0.065 Uiso calc R 1
C C21 0.0764(5) 0.0453(3) 1.1636(3) 0.0528(11) Uani d . 1
H H21 0.1155 0.0176 1.2186 0.063 Uiso calc R 1
C C22 0.1590(5) 0.0943(3) 1.1138(3) 0.0471(10) Uani d . 1
H H22 0.2546 0.0983 1.1367 0.057 Uiso calc R 1
C C23 -0.0285(4) 0.1300(2) 1.0011(3) 0.0387(8) Uani d . 1
C C24 -0.0815(4) 0.1736(2) 0.9152(3) 0.0407(9) Uani d . 1
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
_geom_angle_publ_flag
N1 W Cl2 92.33(9) y
N1 W Cl1 101.41(8) y
N1 W N2 66.71(12) y
N1 W N3 97.12(9) y
N2 W N3 79.72(8) y
N3 W N4 65.32(12) y
N4 W N1 150.19(11) ?
N4 W N2 85.87(11) y
N4 W Cl1 89.88(8) y
N4 W Cl2 109.34(8) y
Cl1 W N2 90.66(8) y
Cl2 W Cl1 111.13(4) y
Cl2 W N2 152.83(8) ?
Cl2 W N3 86.42(9) y
C1 N1 C12 119.1(4) ?
C1 N1 W 122.2(3) ?
C12 N1 W 117.4(3) ?
C10 N2 C11 118.7(4) ?
C10 N2 W 124.1(3) ?
C11 N2 W 116.5(3) ?
C13 N3 C24 118.9(4) ?
C22 N4 C23 118.8(3) ?
C22 N4 W 120.7(3) ?
C23 N4 W 120.5(2) ?
N1 C1 C2 122.1(5) ?
N1 C1 H1 118.9 ?
C2 C1 H1 118.9 ?
C3 C2 C1 119.3(5) ?
C3 C2 H2 120.3 ?
C1 C2 H2 120.3 ?
C2 C3 C4 119.5(5) ?
C2 C3 H3 120.3 ?
C4 C3 H3 120.3 ?
C3 C4 C12 117.7(5) ?
C3 C4 C5 122.2(5) ?
C12 C4 C5 120.0(5) ?
C6 C5 C4 120.3(5) ?
C6 C5 H5 119.8 ?
C4 C5 H5 119.8 ?
C5 C6 C7 122.3(5) ?
C5 C6 H6 118.9 ?
C7 C6 H6 118.9 ?
C8 C7 C11 118.5(4) ?
C8 C7 C6 123.7(5) ?
C11 C7 C6 117.8(5) ?
C9 C8 C7 120.4(4) ?
C9 C8 H8 119.8 ?
C7 C8 H8 119.8 ?
C8 C9 C10 117.9(5) ?
C8 C9 H9 121.0 ?
C10 C9 H9 121.0 ?
N2 C10 C9 123.6(5) ?
N2 C10 H10 118.2 ?
C9 C10 H10 118.2 ?
N2 C11 C7 121.0(4) ?
N2 C11 C12 118.3(3) ?
C7 C11 C12 120.8(4) ?
N1 C12 C4 122.2(4) ?
N1 C12 C11 119.1(3) ?
C4 C12 C11 118.7(4) ?
N3 C13 C14 122.6(5) ?
N3 C13 H13 118.7 ?
C14 C13 H13 118.7 ?
C15 C14 C13 119.2(5) ?
C15 C14 H14 120.4 ?
C13 C14 H14 120.4 ?
C14 C15 C16 119.9(5) ?
C14 C15 H15 120.0 ?
C16 C15 H15 120.0 ?
C15 C16 C24 117.3(5) ?
C15 C16 C17 123.2(4) ?
C24 C16 C17 119.5(4) ?
C18 C17 C16 121.5(4) ?
C18 C17 H17 119.2 ?
C16 C17 H17 119.2 ?
C17 C18 C19 121.0(5) ?
C17 C18 H18 119.5 ?
C19 C18 H18 119.5 ?
C20 C19 C23 118.0(4) ?
C20 C19 C18 122.9(4) ?
C23 C19 C18 119.1(4) ?
C21 C20 C19 119.8(4) ?
C21 C20 H20 120.1 ?
C19 C20 H20 120.1 ?
C20 C21 C22 118.2(4) ?
C20 C21 H21 120.9 ?
C22 C21 H21 120.9 ?
N4 C22 C21 123.7(4) ?
N4 C22 H22 118.1 ?
C21 C22 H22 118.1 ?
N4 C23 C19 121.4(4) ?
N4 C23 C24 118.7(3) ?
C19 C23 C24 120.0(4) ?
N3 C24 C16 122.1(4) ?
N3 C24 C23 118.9(3) ?
C16 C24 C23 119.0(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
W N1 2.488(3) y
W N2 2.524(3) y
W N3 2.582(3) y
W N4 2.477(3) y
W Cl1 2.5183(14) y
W Cl2 2.4922(12) y
N1 C1 1.314(5) ?
N1 C12 1.354(5) ?
N2 C10 1.318(5) ?
N2 C11 1.358(5) ?
N3 C13 1.329(6) ?
N3 C24 1.345(5) ?
N4 C22 1.327(5) ?
N4 C23 1.343(5) ?
C1 C2 1.400(7) ?
C1 H1 0.9300 ?
C2 C3 1.365(8) ?
C2 H2 0.9300 ?
C3 C4 1.395(7) ?
C3 H3 0.9300 ?
C4 C12 1.397(6) ?
C4 C5 1.433(7) ?
C5 C6 1.355(8) ?
C5 H5 0.9300 ?
C6 C7 1.436(7) ?
C6 H6 0.9300 ?
C7 C8 1.389(7) ?
C7 C11 1.402(6) ?
C8 C9 1.356(7) ?
C8 H8 0.9300 ?
C9 C10 1.397(6) ?
C9 H9 0.9300 ?
C10 H10 0.9300 ?
C11 C12 1.455(6) ?
C13 C14 1.390(8) ?
C13 H13 0.9300 ?
C14 C15 1.361(8) ?
C14 H14 0.9300 ?
C15 C16 1.401(7) ?
C15 H15 0.9300 ?
C16 C24 1.411(5) ?
C16 C17 1.430(7) ?
C17 C18 1.341(7) ?
C17 H17 0.9300 ?
C18 C19 1.434(6) ?
C18 H18 0.9300 ?
C19 C20 1.400(6) ?
C19 C23 1.413(5) ?
C20 C21 1.367(6) ?
C20 H20 0.9300 ?
C21 C22 1.386(6) ?
C21 H21 0.9300 ?
C22 H22 0.9300 ?
C23 C24 1.437(5) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30655186
