#------------------------------------------------------------------------------
#$Date: 2016-03-25 12:47:22 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179815 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/11/7011163.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_7011163
loop_
_publ_author_name
'Long, Nicholas J.'
'Parker, David G.'
'Speyer, Paul R.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Synthesis, characterisation and polymerisation of
 vinylbenzene-substituted triazacyclododecanes and their transition
 metal complexes
;
_journal_issue                   10
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2142
_journal_paper_doi               10.1039/b108235n
_journal_year                    2002
_chemical_formula_sum            'C23 H27 N3 O5 W'
_chemical_formula_weight         609.33
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.257(10)
_cell_angle_beta                 97.580(9)
_cell_angle_gamma                109.314(9)
_cell_formula_units_Z            2
_cell_length_a                   8.6898(10)
_cell_length_b                   10.8424(15)
_cell_length_c                   13.733(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.43
_cell_measurement_theta_min      4.74
_cell_volume                     1208.8(3)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5920
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        13.77
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.815
_exptl_absorpt_correction_T_max  0.7772
_exptl_absorpt_correction_T_min  0.4154
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       'platy blocks'
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.206
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.027
_refine_ls_goodness_of_fit_obs   1.051
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_obs          0.0411
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0377P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0982
_refine_ls_wR_factor_obs         0.0914
_reflns_number_observed          4706
_reflns_number_total             5551
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b108235n.txt
_cod_data_source_block           NL9808
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7011163
loop_
_symmetry_equiv_pos_as_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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
W W -0.00617(3) 0.03536(2) 0.20344(2) 0.04037(8) Uani 1 d . .
N1 N -0.2995(7) 0.3975(5) 0.1627(5) 0.0490(12) Uani 1 d . .
C2 C -0.2836(10) 0.2926(7) 0.1035(6) 0.057(2) Uani 1 d . .
H2A H -0.1672(10) 0.3070(7) 0.1042(6) 0.068 Uiso 1 calc R .
H2B H -0.3295(10) 0.2990(7) 0.0361(6) 0.068 Uiso 1 calc R .
C3 C -0.3642(9) 0.1547(7) 0.1334(6) 0.058(2) Uani 1 d . .
H3A H -0.4827(9) 0.1330(7) 0.1187(6) 0.069 Uiso 1 calc R .
H3B H -0.3332(9) 0.0955(7) 0.0932(6) 0.069 Uiso 1 calc R .
C4 C -0.3220(9) 0.1305(6) 0.2401(6) 0.0514(14) Uani 1 d . .
H4A H -0.3598(9) 0.1854(6) 0.2803(6) 0.062 Uiso 1 calc R .
H4B H -0.3819(9) 0.0401(6) 0.2514(6) 0.062 Uiso 1 calc R .
N5 N -0.1422(7) 0.1566(5) 0.2737(4) 0.0414(10) Uani 1 d . .
C6 C -0.1166(12) 0.1619(8) 0.3845(5) 0.058(2) Uani 1 d . .
H6A H -0.0254(12) 0.1317(8) 0.4073(5) 0.070 Uiso 1 calc R .
H6B H -0.2145(12) 0.1028(8) 0.4071(5) 0.070 Uiso 1 calc R .
C7 C -0.0812(13) 0.2983(9) 0.4295(5) 0.066(2) Uani 1 d . .
H7A H -0.1685(13) 0.3312(9) 0.4032(5) 0.079 Uiso 1 calc R .
H7B H -0.0806(13) 0.2937(9) 0.5001(5) 0.079 Uiso 1 calc R .
C8 C 0.0819(12) 0.3923(9) 0.4090(7) 0.071(2) Uani 1 d . .
H8A H 0.1085(12) 0.4727(9) 0.4489(7) 0.085 Uiso 1 calc R .
H8B H 0.1674(12) 0.3544(9) 0.4279(7) 0.085 Uiso 1 calc R .
N9 N 0.0797(8) 0.4231(6) 0.3048(5) 0.0561(14) Uani 1 d . .
C10 C 0.0229(10) 0.5357(7) 0.2825(8) 0.066(2) Uani 1 d . .
H10A H 0.1054(10) 0.6150(7) 0.3133(8) 0.079 Uiso 1 calc R .
H10B H -0.0779(10) 0.5234(7) 0.3103(8) 0.079 Uiso 1 calc R .
C11 C -0.0082(11) 0.5515(8) 0.1733(8) 0.071(2) Uani 1 d . .
H11A H 0.0312(11) 0.4922(8) 0.1389(8) 0.086 Uiso 1 calc R .
H11B H 0.0542(11) 0.6401(8) 0.1589(8) 0.086 Uiso 1 calc R .
C12 C -0.1901(10) 0.5243(8) 0.1351(8) 0.068(2) Uani 1 d . .
H12A H -0.2238(10) 0.5936(8) 0.1604(8) 0.081 Uiso 1 calc R .
H12B H -0.2034(10) 0.5265(8) 0.0639(8) 0.081 Uiso 1 calc R .
C13 C -0.4699(9) 0.3955(7) 0.1512(6) 0.055(2) Uani 1 d . .
H13A H -0.5410(9) 0.3093(7) 0.1650(6) 0.066 Uiso 1 calc R .
H13B H -0.5030(9) 0.4119(7) 0.0836(6) 0.066 Uiso 1 calc R .
C14 C -0.4921(8) 0.4972(7) 0.2193(5) 0.0488(14) Uani 1 d . .
C15 C -0.4513(10) 0.4988(7) 0.3195(6) 0.057(2) Uani 1 d . .
H15A H -0.4105(10) 0.4355(7) 0.3468(6) 0.069 Uiso 1 calc R .
C16 C -0.4702(10) 0.5937(8) 0.3805(6) 0.059(2) Uani 1 d . .
H16A H -0.4450(10) 0.5913(8) 0.4482(6) 0.070 Uiso 1 calc R .
C17 C -0.5267(9) 0.6932(7) 0.3418(6) 0.057(2) Uani 1 d . .
C18 C -0.5673(10) 0.6900(8) 0.2394(6) 0.058(2) Uani 1 d . .
H18A H -0.6064(10) 0.7537(8) 0.2111(6) 0.069 Uiso 1 calc R .
C19 C -0.5502(9) 0.5945(8) 0.1801(6) 0.054(2) Uani 1 d . .
H19A H -0.5780(9) 0.5946(8) 0.1123(6) 0.065 Uiso 1 calc R .
C20 C -0.5451(12) 0.7913(9) 0.4081(7) 0.067(2) Uani 1 d . .
H20A H -0.4999(12) 0.7927(9) 0.4736(7) 0.081 Uiso 1 calc R .
C21 C -0.6184(14) 0.8779(10) 0.3858(8) 0.078(2) Uani 1 d . .
H21A H -0.6658(14) 0.8810(10) 0.3215(8) 0.093 Uiso 1 calc R .
H21B H -0.6229(14) 0.9362(10) 0.4344(8) 0.093 Uiso 1 calc R .
C22 C 0.1269(10) -0.0546(7) 0.1456(6) 0.056(2) Uani 1 d . .
O22 O 0.2074(9) -0.1031(7) 0.1114(5) 0.075(2) Uani 1 d . .
C23 C -0.0633(11) -0.1039(7) 0.3040(6) 0.059(2) Uani 1 d . .
O23 O -0.0889(12) -0.1808(8) 0.3608(7) 0.099(3) Uani 1 d . .
C24 C -0.2073(9) -0.0801(6) 0.1114(5) 0.0496(14) Uani 1 d . .
O24 O -0.3121(9) -0.1499(6) 0.0594(5) 0.077(2) Uani 1 d . .
C25 C 0.0592(9) 0.1779(7) 0.1053(5) 0.0507(14) Uani 1 d . .
O25 O 0.1047(9) 0.2573(6) 0.0527(5) 0.072(2) Uani 1 d . .
C26 C 0.2025(10) 0.1316(7) 0.2937(6) 0.055(2) Uani 1 d . .
O26 O 0.3280(8) 0.1792(7) 0.3414(5) 0.078(2) Uani 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'
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
_geom_angle_publ_flag
C22 W C26 85.8(3) . . ?
C22 W C23 90.6(3) . . ?
C26 W C23 89.1(3) . . ?
C22 W C25 88.9(3) . . ?
C26 W C25 88.9(3) . . ?
C23 W C25 178.0(3) . . ?
C22 W C24 88.3(3) . . ?
C26 W C24 173.3(3) . . ?
C23 W C24 87.7(3) . . ?
C25 W C24 94.3(3) . . ?
C22 W N5 175.1(3) . . ?
C26 W N5 90.0(3) . . ?
C23 W N5 92.0(3) . . ?
C25 W N5 88.3(2) . . ?
C24 W N5 95.9(2) . . ?
C2 N1 C13 111.1(6) . . ?
C2 N1 C12 109.6(7) . . ?
C13 N1 C12 110.4(6) . . ?
N1 C2 C3 116.8(7) . . ?
C4 C3 C2 115.6(6) . . ?
N5 C4 C3 114.8(6) . . ?
C4 N5 C6 107.6(6) . . ?
C4 N5 W 119.8(4) . . ?
C6 N5 W 113.7(4) . . ?
N5 C6 C7 112.8(6) . . ?
C8 C7 C6 112.3(7) . . ?
N9 C8 C7 112.2(6) . . ?
C8 N9 C10 112.4(7) . . ?
N9 C10 C11 112.0(7) . . ?
C10 C11 C12 112.8(7) . . ?
N1 C12 C11 113.8(6) . . ?
N1 C13 C14 112.0(6) . . ?
C15 C14 C19 118.5(7) . . ?
C15 C14 C13 121.6(6) . . ?
C19 C14 C13 119.8(6) . . ?
C14 C15 C16 120.8(7) . . ?
C15 C16 C17 121.3(7) . . ?
C18 C17 C16 117.0(8) . . ?
C18 C17 C20 123.2(7) . . ?
C16 C17 C20 119.8(8) . . ?
C19 C18 C17 121.0(7) . . ?
C18 C19 C14 121.4(7) . . ?
C21 C20 C17 127.3(9) . . ?
O22 C22 W 177.9(7) . . ?
O23 C23 W 177.3(9) . . ?
O24 C24 W 174.9(7) . . ?
O25 C25 W 176.0(7) . . ?
O26 C26 W 173.7(7) . . ?
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
W C22 1.975(8) . ?
W C26 2.014(7) . ?
W C23 2.034(8) . ?
W C25 2.042(7) . ?
W C24 2.043(7) . ?
W N5 2.318(5) . ?
N1 C2 1.449(9) . ?
N1 C13 1.461(9) . ?
N1 C12 1.474(9) . ?
C2 C3 1.511(10) . ?
C3 C4 1.509(10) . ?
C4 N5 1.500(9) . ?
N5 C6 1.508(8) . ?
C6 C7 1.518(10) . ?
C7 C8 1.509(14) . ?
C8 N9 1.470(12) . ?
N9 C10 1.481(10) . ?
C10 C11 1.509(15) . ?
C11 C12 1.527(12) . ?
C13 C14 1.519(10) . ?
C14 C15 1.373(10) . ?
C14 C19 1.394(10) . ?
C15 C16 1.388(12) . ?
C16 C17 1.405(11) . ?
C17 C18 1.402(11) . ?
C17 C20 1.459(12) . ?
C18 C19 1.373(11) . ?
C20 C21 1.315(14) . ?
C22 O22 1.147(10) . ?
C23 O23 1.133(10) . ?
C24 O24 1.132(9) . ?
C25 O25 1.129(9) . ?
C26 O26 1.150(10) . ?
