#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:14:25 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180418 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/87/7208718.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_7208718
loop_
_publ_author_name
'Shizhen, Du'
'Xiaoming, Lu'
'Jun, Feng'
'Yifeng, Cheng'
'Lan, An'
'Xiaojing, Sun'
_publ_section_title
;
 Nano-structures assembled by quantum motifs consisting of tungsten
 complexes and differences from their molybdenum analogues
;
_journal_issue                   20
_journal_name_full               CrystEngComm
_journal_page_first              6618
_journal_paper_doi               10.1039/c2ce25690h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         '4(C12 H8 O6 W), 8(C2 H9 N2), 4(C H4 N)'
_chemical_formula_sum            'C17 H33 N5 O6 W'
_chemical_formula_weight         587.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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                 102.696(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.1354(4)
_cell_length_b                   30.7781(16)
_cell_length_c                   9.8145(5)
_cell_measurement_reflns_used    392
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      26.39
_cell_measurement_theta_min      3.16
_cell_volume                     2102.70(19)
_computing_molecular_graphics
;
OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0212
_diffrn_reflns_av_sigmaI/netI    0.0142
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            19136
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    5.537
_exptl_absorpt_correction_T_max  0.6685
_exptl_absorpt_correction_T_min  0.6512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1998)'
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.091
_refine_ls_extinction_coef       0.00516(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.321
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.321
_refine_ls_R_factor_all          0.0222
_refine_ls_R_factor_gt           0.0214
_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)+(0.0075P)²+3.3614P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0445
_refine_ls_wR_factor_ref         0.0447
_reflns_number_gt                3640
_reflns_number_total             3717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25690h.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               7208718
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y+1/2, -z+1/2'
3 '-x, -y, -z'
4 'x, -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 0.20581(2) 0.647591(4) 0.564509(13) 0.02713(7) Uani 1 1 d .
N1 N 0.7118(5) 0.63488(11) 0.0455(3) 0.0418(8) Uani 1 1 d .
H1A H 0.8340 0.6315 0.0406 0.063 Uiso 1 1 d R
H1C H 0.6418 0.6133 0.0002 0.063 Uiso 1 1 d R
N2 N 0.6738(4) 0.58863(9) 0.3955(3) 0.0326(7) Uani 1 1 d .
H2A H 0.7598 0.6061 0.4480 0.049 Uiso 1 1 calc R
H2B H 0.6894 0.5617 0.4292 0.049 Uiso 1 1 calc R
H2C H 0.5559 0.5978 0.3967 0.049 Uiso 1 1 calc R
N3 N 0.7441(4) 0.50463(10) 0.5155(3) 0.0391(7) Uani 1 1 d .
H3B H 0.6928 0.5053 0.5903 0.059 Uiso 1 1 d R
H3C H 0.6996 0.4816 0.4634 0.059 Uiso 1 1 d R
N6 N 0.6500(6) 0.72501(11) 0.5351(3) 0.0514(9) Uani 1 1 d .
H6A H 0.7027 0.7006 0.5125 0.077 Uiso 1 1 calc R
H6B H 0.6412 0.7442 0.4661 0.077 Uiso 1 1 calc R
H6C H 0.5332 0.7194 0.5488 0.077 Uiso 1 1 calc R
N7 N 0.6435(5) 0.70571(10) 0.8488(3) 0.0375(7) Uani 1 1 d .
H7B H 0.6658 0.6832 0.9069 0.056 Uiso 1 1 d R
H7C H 0.5397 0.7005 0.7820 0.056 Uiso 1 1 d R
O1 O 0.5064(3) 0.63271(8) 0.6107(2) 0.0312(5) Uani 1 1 d .
O2 O 0.2264(4) 0.59436(8) 0.6824(2) 0.0354(6) Uani 1 1 d .
O3 O 0.2159(4) 0.60521(8) 0.3943(2) 0.0388(6) Uani 1 1 d .
O4 O 0.2448(4) 0.68735(7) 0.4151(2) 0.0324(5) Uani 1 1 d .
O5 O 0.2569(4) 0.68974(8) 0.6849(3) 0.0394(6) Uani 1 1 d .
O6 O -0.0441(4) 0.64414(9) 0.5335(3) 0.0413(6) Uani 1 1 d .
C1 C 0.5570(5) 0.59909(11) 0.6965(3) 0.0277(7) Uani 1 1 d .
C2 C 0.4022(5) 0.57763(11) 0.7352(3) 0.0318(8) Uani 1 1 d .
C3 C 0.4344(6) 0.54157(13) 0.8210(4) 0.0440(10) Uani 1 1 d .
H3 H 0.3320 0.5272 0.8455 0.053 Uiso 1 1 calc R
C4 C 0.7429(6) 0.58453(12) 0.7474(4) 0.0365(8) Uani 1 1 d .
H4 H 0.8462 0.5986 0.7231 0.044 Uiso 1 1 calc R
C5 C 0.2154(5) 0.62597(13) 0.2744(4) 0.0338(8) Uani 1 1 d .
C6 C 0.2322(5) 0.67128(12) 0.2845(4) 0.0330(8) Uani 1 1 d .
C7 C 0.2397(5) 0.69692(15) 0.1704(4) 0.0450(10) Uani 1 1 d .
H7 H 0.2530 0.7269 0.1789 0.054 Uiso 1 1 calc R
C8 C 0.2016(6) 0.60615(16) 0.1451(4) 0.0470(10) Uani 1 1 d .
H8 H 0.1885 0.5762 0.1358 0.056 Uiso 1 1 calc R
C9 C 0.7733(7) 0.54846(14) 0.8355(4) 0.0465(10) Uani 1 1 d .
H9 H 0.8978 0.5388 0.8714 0.056 Uiso 1 1 calc R
C10 C 0.6204(7) 0.52697(14) 0.8700(4) 0.0506(11) Uani 1 1 d .
H10 H 0.6426 0.5025 0.9266 0.061 Uiso 1 1 calc R
C11 C 0.2077(6) 0.6323(2) 0.0291(4) 0.0591(14) Uani 1 1 d .
H11 H 0.1985 0.6195 -0.0579 0.071 Uiso 1 1 calc R
C12 C 0.2269(6) 0.6764(2) 0.0423(4) 0.0583(13) Uani 1 1 d .
H12 H 0.2315 0.6930 -0.0360 0.070 Uiso 1 1 calc R
C13 C 0.7007(6) 0.58904(11) 0.2503(4) 0.0334(8) Uani 1 1 d .
H13A H 0.5998 0.5720 0.1919 0.040 Uiso 1 1 calc R
H13B H 0.8227 0.5755 0.2479 0.040 Uiso 1 1 calc R
C14 C 0.6974(5) 0.63425(11) 0.1919(3) 0.0299(7) Uani 1 1 d .
H14A H 0.5789 0.6484 0.2000 0.036 Uiso 1 1 calc R
H14B H 0.8033 0.6507 0.2470 0.036 Uiso 1 1 calc R
C15 C 0.9524(6) 0.50126(14) 0.5610(4) 0.0421(9) Uani 1 1 d .
H15A H 0.9845 0.4755 0.6184 0.050 Uiso 1 1 calc R
H15B H 1.0010 0.5264 0.6176 0.050 Uiso 1 1 calc R
C16 C 0.8110(6) 0.71232(14) 0.7846(4) 0.0457(10) Uani 1 1 d .
H16A H 0.8513 0.6844 0.7549 0.055 Uiso 1 1 calc R
H16B H 0.9168 0.7241 0.8543 0.055 Uiso 1 1 calc R
C18 C 0.7678(6) 0.74261(13) 0.6610(4) 0.0445(10) Uani 1 1 d .
H18A H 0.7045 0.7682 0.6870 0.053 Uiso 1 1 calc R
H18B H 0.8887 0.7520 0.6408 0.053 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'
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_
_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
N1 C14 C13 112.9(3) . .
N1 C14 H14A 109.0 . .
N1 C14 H14B 109.0 . .
H1A N1 H1C 109.5 . .
N2 C13 H13A 109.1 . .
N2 C13 H13B 109.1 . .
N2 C13 C14 112.4(3) . .
H2A N2 H2B 109.5 . .
H2A N2 H2C 109.5 . .
H2B N2 H2C 109.5 . .
N3 C15 C15 111.6(4) . 3_766
N3 C15 H15A 109.3 . .
N3 C15 H15B 109.3 . .
H3B N3 H3C 109.5 . .
N6 C18 C16 115.8(3) . .
N6 C18 H18A 108.3 . .
N6 C18 H18B 108.3 . .
H6A N6 H6B 109.5 . .
H6A N6 H6C 109.5 . .
H6B N6 H6C 109.5 . .
N7 C16 H16A 109.1 . .
N7 C16 H16B 109.1 . .
N7 C16 C18 112.7(3) . .
H7B N7 H7C 109.5 . .
O1 C1 C2 114.5(3) . .
O1 C1 C4 125.7(3) . .
O2 W1 O1 76.03(9) . .
O2 W1 O3 86.62(10) . .
O2 C2 C1 115.8(3) . .
O2 C2 C3 123.8(3) . .
O3 W1 O1 80.23(10) . .
O3 C5 C6 115.4(3) . .
O3 C5 C8 125.3(4) . .
O4 W1 O1 89.53(9) . .
O4 W1 O2 159.35(10) . .
O4 W1 O3 76.30(10) . .
O4 C6 C5 114.6(3) . .
O4 C6 C7 123.4(4) . .
O5 W1 O1 88.00(11) . .
O5 W1 O2 103.95(11) . .
O5 W1 O3 161.88(11) . .
O5 W1 O4 89.98(11) . .
O5 W1 O6 102.57(12) . .
O6 W1 O1 163.99(11) . .
O6 W1 O2 89.63(11) . .
O6 W1 O3 92.02(12) . .
O6 W1 O4 102.31(11) . .
C1 O1 W1 114.8(2) . .
C1 C4 H4 120.4 . .
C1 C4 C9 119.2(4) . .
C2 O2 W1 118.7(2) . .
C2 C3 H3 120.3 . .
C2 C3 C10 119.4(4) . .
C3 C2 C1 120.4(4) . .
C3 C10 H10 119.7 . .
C4 C1 C2 119.8(3) . .
C4 C9 H9 119.7 . .
C5 O3 W1 113.7(2) . .
C5 C8 H8 120.7 . .
C5 C8 C11 118.7(4) . .
C6 O4 W1 118.9(2) . .
C6 C7 H7 121.1 . .
C6 C7 C12 117.8(4) . .
C7 C6 C5 122.0(4) . .
C7 C12 H12 119.3 . .
C8 C5 C6 119.2(4) . .
C8 C11 H11 119.6 . .
C9 C4 H4 120.4 . .
C9 C10 C3 120.6(4) . .
C9 C10 H10 119.7 . .
C10 C3 H3 120.3 . .
C10 C9 C4 120.7(4) . .
C10 C9 H9 119.7 . .
C11 C8 H8 120.7 . .
C11 C12 C7 121.4(4) . .
C11 C12 H12 119.3 . .
C12 C7 H7 121.1 . .
C12 C11 C8 120.9(4) . .
C12 C11 H11 119.6 . .
C13 N2 H2A 109.5 . .
C13 N2 H2B 109.5 . .
C13 N2 H2C 109.5 . .
C13 C14 H14A 109.0 . .
C13 C14 H14B 109.0 . .
H13A C13 H13B 107.9 . .
C14 N1 H1A 109.5 . .
C14 N1 H1C 109.2 . .
C14 C13 H13A 109.1 . .
C14 C13 H13B 109.1 . .
H14A C14 H14B 107.8 . .
C15 N3 H3B 109.0 . .
C15 N3 H3C 109.3 . .
C15 C15 H15A 109.3 3_766 .
C15 C15 H15B 109.3 3_766 .
H15A C15 H15B 108.0 . .
C16 N7 H7B 109.4 . .
C16 N7 H7C 109.2 . .
C16 C18 H18A 108.3 . .
C16 C18 H18B 108.3 . .
H16A C16 H16B 107.8 . .
C18 N6 H6A 109.5 . .
C18 N6 H6B 109.5 . .
C18 N6 H6C 109.5 . .
C18 C16 H16A 109.1 . .
C18 C16 H16B 109.1 . .
H18A C18 H18B 107.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O1 2.142(2) .
W1 O2 1.992(2) .
W1 O3 2.133(2) .
W1 O4 1.976(2) .
W1 O5 1.739(2) .
W1 O6 1.745(3) .
N1 H1A 0.8900 .
N1 H1C 0.8898 .
N1 C14 1.462(4) .
N2 H2A 0.8900 .
N2 H2B 0.8900 .
N2 H2C 0.8900 .
N2 C13 1.479(4) .
N3 H3B 0.8900 .
N3 H3C 0.8901 .
N3 C15 1.459(5) .
N6 H6A 0.8900 .
N6 H6B 0.8900 .
N6 H6C 0.8900 .
N6 C18 1.439(5) .
N7 H7B 0.8899 .
N7 H7C 0.8900 .
N7 C16 1.483(5) .
O1 C1 1.333(4) .
O2 C2 1.350(4) .
O3 C5 1.338(4) .
O4 C6 1.359(4) .
C1 C2 1.409(5) .
C1 C4 1.385(5) .
C2 C3 1.381(5) .
C3 H3 0.9300 .
C3 C10 1.384(6) .
C4 H4 0.9300 .
C4 C9 1.395(5) .
C5 C6 1.401(5) .
C5 C8 1.392(5) .
C6 C7 1.380(5) .
C7 H7 0.9300 .
C7 C12 1.392(6) .
C8 H8 0.9300 .
C8 C11 1.402(7) .
C9 H9 0.9300 .
C9 C10 1.380(6) .
C10 H10 0.9300 .
C11 H11 0.9300 .
C11 C12 1.367(8) .
C12 H12 0.9300 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 C14 1.503(5) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C15 1.502(8) 3_766
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C16 C18 1.508(5) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
