#------------------------------------------------------------------------------
#$Date: 2025-08-18 16:20:24 +0200 (Mon 18 de Aug de 2025) $
#$Revision: 301776 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/29/1512944.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_1512944
loop_
_publ_author_name
'Timothy J. Boyle'
'Leigh Anna M. Ottley'
_publ_section_title
;
 Structural characterization of the coordination behavior of
 4,4'-di-methoxy,2,2'-di-ol-benzophenone modified metal
 alkoxides
;
_journal_issue                   1
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              69
_journal_page_last               80
_journal_paper_doi               10.1016/j.ica.2010.08.047
_journal_volume                  364
_journal_year                    2010
_chemical_formula_moiety         'C40 H34 N2 O14 W2, (C5 H5 N)2'
_chemical_formula_sum            'C50 H44 N4 O14 W2'
_chemical_formula_weight         1172.49
_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-97
_cell_angle_alpha                98.2580(10)
_cell_angle_beta                 107.5770(10)
_cell_angle_gamma                115.9850(10)
_cell_formula_units_Z            1
_cell_length_a                   10.0466(6)
_cell_length_b                   11.4273(7)
_cell_length_c                   12.4642(8)
_cell_measurement_reflns_used    3673
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.85
_cell_measurement_theta_min      2.28
_cell_volume                     1160.93(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0245
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8461
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    5.015
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.624
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.677
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.245
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0294P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                3765
_reflns_number_total             4152
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            2010-69.cif
_cod_data_source_block           10mr102s
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 


  Updating the _chemical_formula_sum to include the pyridine solvate
  carbon atoms (and to match the computed formula). Also adding
  _chemical_formula_moiety singling out the standalone pyridine
  moieties.

  Saulius Gra\<zulis
  2013-12-06

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        1160.93(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C40 H44 N4 O14 W2'
_cod_database_code               1512944
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
W1 W 0.51920(2) 0.673171(18) 0.713869(15) 0.02296(7) Uani 1 1 d .
O1 O 0.7445(3) 0.8193(3) 0.8189(2) 0.0241(7) Uani 1 1 d .
N1 N 0.5861(4) 0.8044(4) 0.5888(3) 0.0236(8) Uani 1 1 d .
C9 C 0.2243(5) 0.5476(4) 0.4768(4) 0.0200(9) Uani 1 1 d .
O2 O 0.4911(4) 0.5599(3) 0.7932(3) 0.0349(8) Uani 1 1 d .
C10 C 0.1756(5) 0.6398(4) 0.5040(4) 0.0217(9) Uani 1 1 d .
H10 H 0.2322 0.7065 0.5808 0.026 Uiso 1 1 calc R
C11 C 0.0447(5) 0.6356(4) 0.4202(4) 0.0246(10) Uani 1 1 d .
C17 C 0.6445(5) 0.9406(5) 0.6299(4) 0.0290(10) Uani 1 1 d .
H17 H 0.6564 0.9788 0.7075 0.035 Uiso 1 1 calc R
C4 C 1.1844(5) 0.9907(4) 0.7920(4) 0.0271(10) Uani 1 1 d .
H4 H 1.2880 1.0312 0.7894 0.032 Uiso 1 1 calc R
O3 O 0.4369(4) 0.7656(3) 0.7556(3) 0.0315(7) Uani 1 1 d .
C1 C 0.8842(5) 0.8719(4) 0.8056(3) 0.0220(9) Uani 1 1 d .
C20 C 0.6072(6) 0.8322(5) 0.4073(4) 0.0348(11) Uani 1 1 d .
H20 H 0.5926 0.7921 0.3293 0.042 Uiso 1 1 calc R
C21 C 0.5680(5) 0.7524(5) 0.4782(4) 0.0278(10) Uani 1 1 d .
H21 H 0.5264 0.6566 0.4477 0.033 Uiso 1 1 calc R
C12 C -0.0388(5) 0.5402(4) 0.3070(4) 0.0264(10) Uani 1 1 d .
H12 H -0.1270 0.5385 0.2490 0.032 Uiso 1 1 calc R
C3 C 1.1406(5) 1.0721(4) 0.8512(4) 0.0248(10) Uani 1 1 d .
C5 C 1.0779(5) 0.8537(4) 0.7385(4) 0.0268(10) Uani 1 1 d .
H5 H 1.1086 0.7996 0.6980 0.032 Uiso 1 1 calc R
C18 C 0.6873(6) 1.0259(5) 0.5649(4) 0.0353(12) Uani 1 1 d .
H18 H 0.7298 1.1216 0.5975 0.042 Uiso 1 1 calc R
C14 C 0.1416(5) 0.4494(4) 0.3629(4) 0.0209(9) Uani 1 1 d .
C19 C 0.6682(6) 0.9717(5) 0.4515(5) 0.0407(13) Uani 1 1 d .
H19 H 0.6964 1.0293 0.4045 0.049 Uiso 1 1 calc R
O7 O 0.3455(3) 0.5445(3) 0.5610(2) 0.0220(6) Uani 1 1 d .
O4 O 0.6560(3) 0.5969(3) 0.6474(2) 0.0244(7) Uani 1 1 d .
O5 O 0.0091(4) 0.7311(3) 0.4597(3) 0.0292(7) Uani 1 1 d .
O6 O 1.2504(4) 1.2083(3) 0.8942(3) 0.0353(8) Uani 1 1 d .
C15 C 0.1948(5) 0.3551(4) 0.3259(4) 0.0230(9) Uani 1 1 d .
C6 C 0.9231(5) 0.7888(4) 0.7409(4) 0.0217(9) Uani 1 1 d .
C2 C 0.9935(5) 1.0125(4) 0.8595(4) 0.0249(10) Uani 1 1 d .
H2 H 0.9662 1.0678 0.9023 0.030 Uiso 1 1 calc R
C13 C 0.0100(5) 0.4477(4) 0.2808(4) 0.0258(10) Uani 1 1 d .
H13 H -0.0482 0.3805 0.2042 0.031 Uiso 1 1 calc R
C7 C 1.2103(6) 1.3004(5) 0.9467(4) 0.0406(12) Uani 1 1 d .
H7A H 1.1063 1.2842 0.8912 0.061 Uiso 1 1 calc R
H7B H 1.2953 1.3954 0.9648 0.061 Uiso 1 1 calc R
H7C H 1.2016 1.2850 1.0203 0.061 Uiso 1 1 calc R
C16 C -0.1094(6) 0.7476(5) 0.3763(5) 0.0414(13) Uani 1 1 d .
H16A H -0.0779 0.7674 0.3110 0.062 Uiso 1 1 calc R
H16B H -0.1163 0.8239 0.4161 0.062 Uiso 1 1 calc R
H16C H -0.2154 0.6628 0.3447 0.062 Uiso 1 1 calc R
C26 C 0.2801(7) 0.8569(6) 0.0451(5) 0.0510(14) Uani 1 1 d .
H26 H 0.2750 0.9344 0.0302 0.061 Uiso 1 1 calc R
C25 C 0.3537(7) 0.8087(6) -0.0092(5) 0.0520(15) Uani 1 1 d .
H25 H 0.3956 0.8503 -0.0612 0.062 Uiso 1 1 calc R
C24 C 0.3659(7) 0.6997(6) 0.0128(5) 0.0539(16) Uani 1 1 d .
H24 H 0.4166 0.6637 -0.0234 0.065 Uiso 1 1 calc R
C22 C 0.2282(8) 0.6971(6) 0.1368(6) 0.0666(19) Uani 1 1 d .
H22 H 0.1828 0.6560 0.1876 0.080 Uiso 1 1 calc R
C23 C 0.3033(8) 0.6435(6) 0.0881(6) 0.0659(19) Uani 1 1 d .
H23 H 0.3115 0.5684 0.1066 0.079 Uiso 1 1 calc R
N2 N 0.2159(6) 0.8045(5) 0.1161(4) 0.0571(13) 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'
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
O3 W1 O2 104.15(15) . .
O3 W1 O7 100.88(13) . .
O2 W1 O7 97.70(13) . .
O3 W1 O1 93.76(13) . .
O2 W1 O1 99.74(13) . .
O7 W1 O1 153.71(12) . .
O3 W1 O4 166.26(13) . .
O2 W1 O4 88.76(13) . .
O7 W1 O4 81.69(11) . .
O1 W1 O4 79.19(11) . .
O3 W1 N1 88.89(13) . .
O2 W1 N1 166.96(13) . .
O7 W1 N1 79.71(11) . .
O1 W1 N1 78.87(12) . .
O4 W1 N1 78.24(11) . .
C1 O1 W1 133.8(3) . .
C21 N1 C17 117.5(4) . .
C21 N1 W1 124.4(3) . .
C17 N1 W1 118.1(3) . .
O7 C9 C10 121.0(4) . .
O7 C9 C14 119.0(3) . .
C10 C9 C14 119.8(4) . .
C9 C10 C11 120.6(4) . .
C9 C10 H10 119.7 . .
C11 C10 H10 119.7 . .
O5 C11 C10 114.2(4) . .
O5 C11 C12 125.0(4) . .
C10 C11 C12 120.8(4) . .
N1 C17 C18 122.8(4) . .
N1 C17 H17 118.6 . .
C18 C17 H17 118.6 . .
C5 C4 C3 119.6(4) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
O1 C1 C2 117.9(4) . .
O1 C1 C6 121.9(4) . .
C2 C1 C6 120.2(4) . .
C21 C20 C19 118.8(4) . .
C21 C20 H20 120.6 . .
C19 C20 H20 120.6 . .
N1 C21 C20 122.8(4) . .
N1 C21 H21 118.6 . .
C20 C21 H21 118.6 . .
C13 C12 C11 118.2(4) . .
C13 C12 H12 120.9 . .
C11 C12 H12 120.9 . .
O6 C3 C2 124.9(4) . .
O6 C3 C4 114.9(4) . .
C2 C3 C4 120.2(4) . .
C4 C5 C6 122.2(4) . .
C4 C5 H5 118.9 . .
C6 C5 H5 118.9 . .
C17 C18 C19 119.3(4) . .
C17 C18 H18 120.3 . .
C19 C18 H18 120.3 . .
C13 C14 C9 118.1(4) . .
C13 C14 C15 119.5(4) . .
C9 C14 C15 122.4(4) . .
C18 C19 C20 118.8(5) . .
C18 C19 H19 120.6 . .
C20 C19 H19 120.6 . .
C9 O7 W1 134.3(2) . .
C15 O4 W1 133.0(3) 2_666 .
C11 O5 C16 118.7(3) . .
C3 O6 C7 118.9(4) . .
O4 C15 C6 121.4(4) 2_666 2_666
O4 C15 C14 118.3(4) 2_666 .
C6 C15 C14 120.4(4) 2_666 .
C5 C6 C1 117.2(4) . .
C5 C6 C15 121.5(4) . 2_666
C1 C6 C15 121.3(4) . 2_666
C3 C2 C1 120.5(4) . .
C3 C2 H2 119.8 . .
C1 C2 H2 119.8 . .
C12 C13 C14 122.4(4) . .
C12 C13 H13 118.8 . .
C14 C13 H13 118.8 . .
O6 C7 H7A 109.5 . .
O6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
O6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
O5 C16 H16A 109.5 . .
O5 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
O5 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
N2 C26 C25 125.0(6) . .
N2 C26 H26 117.5 . .
C25 C26 H26 117.5 . .
C24 C25 C26 118.6(6) . .
C24 C25 H25 120.7 . .
C26 C25 H25 120.7 . .
C25 C24 C23 118.3(5) . .
C25 C24 H24 120.8 . .
C23 C24 H24 120.8 . .
N2 C22 C23 123.2(6) . .
N2 C22 H22 118.4 . .
C23 C22 H22 118.4 . .
C24 C23 C22 119.0(6) . .
C24 C23 H23 120.5 . .
C22 C23 H23 120.5 . .
C26 N2 C22 115.8(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
W1 O3 1.714(3) .
W1 O2 1.717(3) .
W1 O7 1.943(3) .
W1 O1 1.974(3) .
W1 O4 2.206(3) .
W1 N1 2.356(4) .
O1 C1 1.337(5) .
N1 C21 1.343(5) .
N1 C17 1.349(5) .
C9 O7 1.364(5) .
C9 C10 1.383(5) .
C9 C14 1.406(6) .
C10 C11 1.387(6) .
C10 H10 0.9500 .
C11 O5 1.362(5) .
C11 C12 1.387(6) .
C17 C18 1.365(6) .
C17 H17 0.9500 .
C4 C5 1.357(6) .
C4 C3 1.399(6) .
C4 H4 0.9500 .
C1 C2 1.392(6) .
C1 C6 1.415(6) .
C20 C21 1.377(6) .
C20 C19 1.381(6) .
C20 H20 0.9500 .
C21 H21 0.9500 .
C12 C13 1.384(6) .
C12 H12 0.9500 .
C3 O6 1.351(5) .
C3 C2 1.375(6) .
C5 C6 1.412(6) .
C5 H5 0.9500 .
C18 C19 1.378(7) .
C18 H18 0.9500 .
C14 C13 1.396(6) .
C14 C15 1.474(6) .
C19 H19 0.9500 .
O4 C15 1.259(5) 2_666
O5 C16 1.428(5) .
O6 C7 1.426(5) .
C15 O4 1.259(5) 2_666
C15 C6 1.450(6) 2_666
C6 C15 1.450(6) 2_666
C2 H2 0.9500 .
C13 H13 0.9500 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C16 H16A 0.9800 .
C16 H16B 0.9800 .
C16 H16C 0.9800 .
C26 N2 1.310(7) .
C26 C25 1.364(8) .
C26 H26 0.9500 .
C25 C24 1.360(8) .
C25 H25 0.9500 .
C24 C23 1.366(8) .
C24 H24 0.9500 .
C22 N2 1.339(7) .
C22 C23 1.374(8) .
C22 H22 0.9500 .
C23 H23 0.9500 .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139041578
