#------------------------------------------------------------------------------
#$Date: 2020-05-16 04:59:56 +0300 (Sat, 16 May 2020) $
#$Revision: 252072 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240538.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_7240538
loop_
_publ_author_name
'Hodorowicz, Maciej'
'Szklarzewicz, Janusz'
'Jurowska, Anna'
_publ_section_title
;
 The versatility of lithium cation coordination modes in salts with
 [W(CN)6(bpy)]2- anion
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00468E
_journal_year                    2020
_chemical_formula_sum            'C16 H8 Cl Li3 N8 O2 W'
_chemical_formula_weight         584.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-04-05 deposited with the CCDC.	2020-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                94.505(2)
_cell_angle_beta                 95.182(2)
_cell_angle_gamma                95.941(2)
_cell_formula_units_Z            2
_cell_length_a                   9.2897(2)
_cell_length_b                   9.4735(2)
_cell_length_c                   13.3937(3)
_cell_measurement_reflns_used    22288
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      27.5990
_cell_measurement_theta_min      3.3070
_cell_volume                     1163.00(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXL-2017/1 (Sheldrick, 2017)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      130.10(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3756
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0527
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51463
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.706
_diffrn_reflns_theta_min         3.066
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.107
_exptl_absorpt_correction_T_max  0.07245
_exptl_absorpt_correction_T_min  0.04730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       prism
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.707
_refine_diff_density_min         -2.080
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         5760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0356
_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)+(0.0488P)²+3.8817P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5087
_reflns_number_total             5760
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00468e1.cif
_cod_data_source_block           shelx
_cod_database_code               7240538
_shelx_shelxl_version_number     2017/1
_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   0.428
_shelx_estimated_absorpt_t_max   0.629
_exptl_absorpt_special_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
W1 W 0.12790(2) 0.29759(2) 0.26018(2) 0.02047(7) Uani 1 1 d . . . . .
N1 N 0.2212(5) 0.4475(5) 0.3915(4) 0.0345(11) Uani 1 1 d . . . . .
N16 N 0.0365(6) -0.0413(5) 0.1837(4) 0.0398(12) Uani 1 1 d . . . . .
N17 N 0.0765(6) 0.6171(5) 0.1904(4) 0.0384(11) Uani 1 1 d . . . . .
N12 N 0.0136(5) 0.2336(5) 0.3914(3) 0.0309(10) Uani 1 1 d . . . . .
C18 C -0.0991(6) 0.3063(7) 0.2165(4) 0.0343(12) Uani 1 1 d . . . . .
C4 C 0.3452(11) 0.6107(9) 0.5655(7) 0.081(4) Uani 1 1 d . . . . .
H4 H 0.388707 0.666093 0.624805 0.098 Uiso 1 1 calc R U . . .
N13 N 0.3638(5) 0.1172(5) 0.3834(4) 0.0382(11) Uani 1 1 d . . . . .
C11 C -0.0972(6) 0.1284(7) 0.3866(5) 0.0412(14) Uani 1 1 d . . . . .
H11 H -0.133130 0.081510 0.322537 0.049 Uiso 1 1 calc R U . . .
N18 N -0.2199(6) 0.3121(8) 0.1934(5) 0.0550(17) Uani 1 1 d . . . . .
C2 C 0.3227(8) 0.5572(6) 0.3869(6) 0.0479(17) Uani 1 1 d . . . . .
H2 H 0.352663 0.578695 0.323295 0.057 Uiso 1 1 calc R U . . .
C16 C 0.0676(6) 0.0777(6) 0.2095(4) 0.0269(10) Uani 1 1 d . . . . .
N14 N 0.4471(5) 0.3861(7) 0.1829(4) 0.0441(13) Uani 1 1 d . . . . .
C5 C 0.2408(11) 0.4993(9) 0.5710(6) 0.068(3) Uani 1 1 d . . . . .
H5 H 0.211070 0.477202 0.634514 0.082 Uiso 1 1 calc R U . . .
C10 C -0.1605(8) 0.0857(10) 0.4695(6) 0.061(2) Uani 1 1 d . . . . .
H10 H -0.238854 0.011623 0.462077 0.074 Uiso 1 1 calc R U . . .
C3 C 0.3855(10) 0.6408(8) 0.4735(7) 0.068(3) Uani 1 1 d . . . . .
H3 H 0.456581 0.718859 0.468261 0.082 Uiso 1 1 calc R U . . .
C17 C 0.0954(6) 0.5079(6) 0.2156(4) 0.0290(11) Uani 1 1 d . . . . .
C6 C 0.1778(8) 0.4180(7) 0.4836(4) 0.0429(16) Uani 1 1 d . . . . .
C13 C 0.2823(5) 0.1786(5) 0.3399(4) 0.0257(10) Uani 1 1 d . . . . .
C7 C 0.0622(7) 0.3001(8) 0.4832(4) 0.0416(15) Uani 1 1 d . . . . .
N15 N 0.1008(5) 0.2627(5) 0.0116(3) 0.0338(10) Uani 1 1 d . . . . .
C15 C 0.1097(5) 0.2733(5) 0.0977(4) 0.0258(10) Uani 1 1 d . . . . .
C14 C 0.3358(6) 0.3556(6) 0.2100(4) 0.0291(11) Uani 1 1 d . . . . .
C8 C 0.0022(10) 0.2597(11) 0.5702(5) 0.064(3) Uani 1 1 d . . . . .
H8 H 0.038039 0.306759 0.634233 0.077 Uiso 1 1 calc R U . . .
C9 C -0.1112(9) 0.1489(12) 0.5614(6) 0.074(3) Uani 1 1 d . . . . .
H9 H -0.152816 0.118809 0.619472 0.089 Uiso 1 1 calc R U . . .
Li1 Li -0.0590(11) 0.7604(10) 0.1404(7) 0.0315(19) Uani 1 1 d . . . . .
Cl1 Cl -0.28490(19) 0.7085(2) 0.20908(14) 0.0556(5) Uani 1 1 d . . . . .
O1 O -0.3506(7) 0.4614(9) 0.0074(5) 0.090(2) Uani 1 1 d . . . . .
O2 O -0.4197(10) 0.0694(11) 0.2065(10) 0.145(4) Uani 1 1 d . . . . .
Li3 Li -0.3467(10) 0.1949(14) -0.1142(10) 0.051(3) Uani 1 1 d . . . . .
Li2 Li -0.3554(13) 0.4613(16) 0.1485(11) 0.061(4) Uani 1 1 d . . . . .
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'
W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C14 W1 C16 106.8(2) . . ?
C14 W1 C18 140.3(2) . . ?
C16 W1 C18 81.2(2) . . ?
C14 W1 C15 70.8(2) . . ?
C16 W1 C15 70.89(19) . . ?
C18 W1 C15 75.8(2) . . ?
C14 W1 C17 80.7(2) . . ?
C16 W1 C17 140.25(19) . . ?
C18 W1 C17 70.5(2) . . ?
C15 W1 C17 75.40(19) . . ?
C14 W1 C13 72.76(19) . . ?
C16 W1 C13 73.50(19) . . ?
C18 W1 C13 144.1(2) . . ?
C15 W1 C13 117.52(19) . . ?
C17 W1 C13 143.05(19) . . ?
C14 W1 N1 81.7(2) . . ?
C16 W1 N1 144.31(18) . . ?
C18 W1 N1 114.8(2) . . ?
C15 W1 N1 142.03(19) . . ?
C17 W1 N1 74.70(18) . . ?
C13 W1 N1 76.40(17) . . ?
C14 W1 N12 144.37(18) . . ?
C16 W1 N12 81.80(19) . . ?
C18 W1 N12 74.50(18) . . ?
C15 W1 N12 142.13(19) . . ?
C17 W1 N12 115.12(19) . . ?
C13 W1 N12 77.06(17) . . ?
N1 W1 N12 73.10(19) . . ?
C2 N1 C6 118.8(6) . . ?
C2 N1 W1 124.2(5) . . ?
C6 N1 W1 116.8(4) . . ?
C16 N16 Li1 168.4(6) . 1_545 ?
C17 N17 Li1 151.3(6) . . ?
C11 N12 C7 117.4(5) . . ?
C11 N12 W1 124.5(4) . . ?
C7 N12 W1 118.0(4) . . ?
N18 C18 W1 179.5(7) . . ?
C3 C4 C5 118.9(7) . . ?
C3 C4 H4 120.6 . . ?
C5 C4 H4 120.6 . . ?
N12 C11 C10 123.3(7) . . ?
N12 C11 H11 118.3 . . ?
C10 C11 H11 118.3 . . ?
C18 N18 Li2 138.8(7) . . ?
N1 C2 C3 121.5(8) . . ?
N1 C2 H2 119.3 . . ?
C3 C2 H2 119.3 . . ?
N16 C16 W1 178.8(5) . . ?
C14 N14 Li2 172.6(8) . 1_655 ?
C4 C5 C6 120.2(9) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C9 C10 C11 119.8(8) . . ?
C9 C10 H10 120.1 . . ?
C11 C10 H10 120.1 . . ?
C4 C3 C2 120.1(9) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
N17 C17 W1 178.5(5) . . ?
N1 C6 C5 120.5(8) . . ?
N1 C6 C7 116.2(5) . . ?
C5 C6 C7 123.3(7) . . ?
N13 C13 W1 178.9(5) . . ?
N12 C7 C8 121.5(7) . . ?
N12 C7 C6 115.2(5) . . ?
C8 C7 C6 123.3(7) . . ?
C15 N15 Li1 173.1(6) . 2_565 ?
N15 C15 W1 178.9(5) . . ?
N14 C14 W1 179.7(6) . . ?
C9 C8 C7 118.9(7) . . ?
C9 C8 H8 120.5 . . ?
C7 C8 H8 120.5 . . ?
C10 C9 C8 119.0(6) . . ?
C10 C9 H9 120.5 . . ?
C8 C9 H9 120.5 . . ?
N16 Li1 N15 109.3(5) 1_565 2_565 ?
N16 Li1 N17 108.7(5) 1_565 . ?
N15 Li1 N17 111.5(5) 2_565 . ?
N16 Li1 Cl1 113.0(5) 1_565 . ?
N15 Li1 Cl1 107.2(4) 2_565 . ?
N17 Li1 Cl1 107.1(4) . . ?
Li1 Cl1 Li2 102.8(4) . . ?
O1 Li2 N14 111.1(7) . 1_455 ?
O1 Li2 N18 105.8(8) . . ?
N14 Li2 N18 104.9(6) 1_455 . ?
O1 Li2 Cl1 103.3(6) . . ?
N14 Li2 Cl1 113.5(7) 1_455 . ?
N18 Li2 Cl1 118.0(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
W1 C14 2.134(5) . ?
W1 C16 2.141(5) . ?
W1 C18 2.149(5) . ?
W1 C15 2.160(5) . ?
W1 C17 2.167(5) . ?
W1 C13 2.171(5) . ?
W1 N1 2.222(4) . ?
W1 N12 2.226(4) . ?
N1 C2 1.338(9) . ?
N1 C6 1.373(8) . ?
N16 C16 1.152(7) . ?
N16 Li1 2.010(10) 1_545 ?
N17 C17 1.139(7) . ?
N17 Li1 2.054(10) . ?
N12 C11 1.350(8) . ?
N12 C7 1.354(8) . ?
C18 N18 1.145(7) . ?
C4 C3 1.363(15) . ?
C4 C5 1.369(15) . ?
C4 H4 0.9500 . ?
N13 C13 1.147(7) . ?
C11 C10 1.372(8) . ?
C11 H11 0.9500 . ?
N18 Li2 2.076(14) . ?
C2 C3 1.397(9) . ?
C2 H2 0.9500 . ?
N14 C14 1.144(7) . ?
N14 Li2 2.005(13) 1_655 ?
C5 C6 1.395(9) . ?
C5 H5 0.9500 . ?
C10 C9 1.345(14) . ?
C10 H10 0.9500 . ?
C3 H3 0.9500 . ?
C6 C7 1.467(11) . ?
C7 C8 1.399(9) . ?
N15 C15 1.145(7) . ?
N15 Li1 2.028(10) 2_565 ?
C8 C9 1.398(14) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
Li1 Cl1 2.387(10) . ?
Cl1 Li2 2.420(16) . ?
O1 Li2 1.894(16) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C5 H5 Cl1 0.95 2.92 3.685(9) 138.5 2_566 yes
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 N12 C11 C10 -0.7(8) . . . . ?
W1 N12 C11 C10 176.2(5) . . . . ?
C6 N1 C2 C3 0.5(9) . . . . ?
W1 N1 C2 C3 -174.8(5) . . . . ?
C3 C4 C5 C6 0.3(10) . . . . ?
N12 C11 C10 C9 -0.6(10) . . . . ?
C5 C4 C3 C2 -1.1(11) . . . . ?
N1 C2 C3 C4 0.7(10) . . . . ?
C2 N1 C6 C5 -1.3(8) . . . . ?
W1 N1 C6 C5 174.3(4) . . . . ?
C2 N1 C6 C7 177.6(5) . . . . ?
W1 N1 C6 C7 -6.8(6) . . . . ?
C4 C5 C6 N1 0.9(9) . . . . ?
C4 C5 C6 C7 -177.9(6) . . . . ?
C11 N12 C7 C8 1.3(8) . . . . ?
W1 N12 C7 C8 -175.8(4) . . . . ?
C11 N12 C7 C6 -177.2(5) . . . . ?
W1 N12 C7 C6 5.6(6) . . . . ?
N1 C6 C7 N12 0.8(7) . . . . ?
C5 C6 C7 N12 179.7(5) . . . . ?
N1 C6 C7 C8 -177.7(5) . . . . ?
C5 C6 C7 C8 1.2(9) . . . . ?
N12 C7 C8 C9 -0.6(9) . . . . ?
C6 C7 C8 C9 177.8(6) . . . . ?
C11 C10 C9 C8 1.4(11) . . . . ?
C7 C8 C9 C10 -0.8(10) . . . . ?
