#------------------------------------------------------------------------------
#$Date: 2025-08-21 12:25:49 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301846 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007274.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_7007274
loop_
_publ_author_name
'Cole, Marcus L.'
'Junk, Peter C.'
'Proctor, Kathryn M.'
'Scott, Janet L.'
'Strauss, Christopher R.'
_publ_section_title
;
 Synthesis and structural characterisation of lithium and sodium
 2,6-dibenzylphenolate complexes.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3338
_journal_page_last               3349
_journal_paper_doi               10.1039/b602706g
_journal_year                    2006
_chemical_compound_source        DME
_chemical_formula_moiety         'C52 H62 Li2 O10'
_chemical_formula_sum            'C52 H62 Li2 O10'
_chemical_formula_weight         860.90
_chemical_melting_point          355
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                97.659(9)
_cell_angle_beta                 112.495(9)
_cell_angle_gamma                94.353(13)
_cell_formula_units_Z            1
_cell_length_a                   9.6584(13)
_cell_length_b                   10.738(2)
_cell_length_c                   12.246(2)
_cell_measurement_temperature    123(2)
_cell_volume                     1151.7(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        X-Seed
_computing_molecular_graphics    'X-Seed / POV-Ray'
_computing_publication_material  'Microsoft Office 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'psi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2389
_diffrn_reflns_av_sigmaI/netI    0.2203
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16328
_diffrn_reflns_theta_full        27.94
_diffrn_reflns_theta_max         27.94
_diffrn_reflns_theta_min         3.98
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.9917
_exptl_absorpt_correction_T_min  0.9834
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'performed as part of the DENZO-SMN package'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.2644
_refine_ls_R_factor_gt           0.0965
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0986P)²+0.3450P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1970
_refine_ls_wR_factor_ref         0.2690
_reflns_number_gt                1988
_reflns_number_total             5327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602706g.txt
_cod_data_source_block           COMPOUND_4
_cod_original_cell_volume        1151.7(4)
_cod_database_code               7007274
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
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.1223(3) 0.0958(3) 0.0554(3) 0.0284(8) Uani 1 1 d . . .
O2 O -0.0080(4) 0.4556(3) -0.1551(3) 0.0477(10) Uani 1 1 d . . .
O3 O 0.4904(4) 0.3111(3) 0.4987(3) 0.0520(10) Uani 1 1 d . . .
O4 O -0.2720(4) 0.1705(3) -0.0547(3) 0.0400(9) Uani 1 1 d . . .
O5 O -0.1419(4) 0.1059(3) 0.1653(3) 0.0420(9) Uani 1 1 d . . .
C1 C 0.2381(5) 0.1868(4) 0.0828(4) 0.0253(10) Uani 1 1 d . . .
C2 C 0.2425(5) 0.2618(4) -0.0037(4) 0.0275(11) Uani 1 1 d . . .
C3 C 0.3603(5) 0.3580(4) 0.0274(4) 0.0280(11) Uani 1 1 d . . .
H3 H 0.3628 0.4075 -0.0308 0.034 Uiso 1 1 calc R . .
C4 C 0.4754(5) 0.3845(4) 0.1412(4) 0.0277(11) Uani 1 1 d . . .
H4 H 0.5547 0.4526 0.1616 0.033 Uiso 1 1 calc R . .
C5 C 0.4732(5) 0.3104(4) 0.2247(4) 0.0286(11) Uani 1 1 d . . .
H5 H 0.5524 0.3278 0.3026 0.034 Uiso 1 1 calc R . .
C6 C 0.3572(5) 0.2103(4) 0.1975(4) 0.0262(10) Uani 1 1 d . . .
C7 C 0.1135(6) 0.2304(4) -0.1265(4) 0.0328(12) Uani 1 1 d . . .
H7A H 0.1071 0.1398 -0.1593 0.039 Uiso 1 1 calc R . .
H7B H 0.0178 0.2418 -0.1169 0.039 Uiso 1 1 calc R . .
C8 C 0.1258(6) 0.3077(5) -0.2161(4) 0.0377(12) Uani 1 1 d . . .
C9 C 0.0662(6) 0.4213(5) -0.2304(4) 0.0361(12) Uani 1 1 d . . .
C10 C 0.0783(6) 0.4929(5) -0.3115(4) 0.0419(13) Uani 1 1 d . . .
H10 H 0.0367 0.5703 -0.3182 0.050 Uiso 1 1 calc R . .
C11 C 0.1543(7) 0.4498(6) -0.3856(5) 0.0545(17) Uani 1 1 d . . .
H11 H 0.1644 0.4975 -0.4427 0.065 Uiso 1 1 calc R . .
C12 C 0.2123(7) 0.3377(6) -0.3724(5) 0.0579(17) Uani 1 1 d . . .
H12 H 0.2627 0.3072 -0.4217 0.070 Uiso 1 1 calc R . .
C13 C 0.1994(6) 0.2689(5) -0.2902(5) 0.0492(15) Uani 1 1 d . . .
H13 H 0.2420 0.1920 -0.2831 0.059 Uiso 1 1 calc R . .
C14 C -0.0701(7) 0.5720(5) -0.1616(6) 0.0604(17) Uani 1 1 d . . .
H14A H 0.0118 0.6430 -0.1359 0.091 Uiso 1 1 calc R . .
H14B H -0.1251 0.5808 -0.1089 0.091 Uiso 1 1 calc R . .
H14C H -0.1397 0.5721 -0.2445 0.091 Uiso 1 1 calc R . .
C15 C 0.3516(5) 0.1318(4) 0.2904(4) 0.0348(12) Uani 1 1 d . . .
H15A H 0.2874 0.1690 0.3292 0.042 Uiso 1 1 calc R . .
H15B H 0.3012 0.0452 0.2482 0.042 Uiso 1 1 calc R . .
C16 C 0.5022(6) 0.1210(4) 0.3878(4) 0.0317(11) Uani 1 1 d . . .
C17 C 0.5725(6) 0.2163(5) 0.4921(4) 0.0355(12) Uani 1 1 d . . .
C18 C 0.7127(6) 0.2087(5) 0.5770(5) 0.0467(14) Uani 1 1 d . . .
H18 H 0.7595 0.2738 0.6455 0.056 Uiso 1 1 calc R . .
C19 C 0.7856(7) 0.1057(5) 0.5625(5) 0.0497(15) Uani 1 1 d . . .
H19 H 0.8833 0.1022 0.6212 0.060 Uiso 1 1 calc R . .
C20 C 0.7224(7) 0.0099(5) 0.4674(5) 0.0495(15) Uani 1 1 d . . .
H20 H 0.7726 -0.0616 0.4606 0.059 Uiso 1 1 calc R . .
C21 C 0.5790(6) 0.0191(5) 0.3781(5) 0.0417(13) Uani 1 1 d . . .
H21 H 0.5344 -0.0464 0.3097 0.050 Uiso 1 1 calc R . .
C22 C 0.5582(8) 0.4106(6) 0.6015(5) 0.074(2) Uani 1 1 d . . .
H22A H 0.5814 0.3745 0.6749 0.111 Uiso 1 1 calc R . .
H22B H 0.4879 0.4725 0.5984 0.111 Uiso 1 1 calc R . .
H22C H 0.6518 0.4528 0.6015 0.111 Uiso 1 1 calc R . .
C23 C -0.2928(7) 0.2976(5) -0.0717(6) 0.0566(16) Uani 1 1 d . . .
H23A H -0.3955 0.2987 -0.1305 0.085 Uiso 1 1 calc R . .
H23B H -0.2192 0.3314 -0.1013 0.085 Uiso 1 1 calc R . .
H23C H -0.2779 0.3500 0.0048 0.085 Uiso 1 1 calc R . .
C24 C -0.3639(6) 0.1196(5) 0.0022(5) 0.0423(13) Uani 1 1 d . . .
H24A H -0.3881 0.0265 -0.0243 0.051 Uiso 1 1 calc R . .
H24B H -0.4602 0.1559 -0.0229 0.051 Uiso 1 1 calc R . .
C25 C -0.2849(6) 0.1491(5) 0.1356(5) 0.0434(13) Uani 1 1 d . . .
H25A H -0.2718 0.2416 0.1644 0.052 Uiso 1 1 calc R . .
H25B H -0.3443 0.1054 0.1732 0.052 Uiso 1 1 calc R . .
C26 C -0.0562(6) 0.1238(5) 0.2903(5) 0.0459(14) Uani 1 1 d . . .
H26A H -0.0450 0.2134 0.3252 0.069 Uiso 1 1 calc R . .
H26B H 0.0440 0.0985 0.3054 0.069 Uiso 1 1 calc R . .
H26C H -0.1081 0.0718 0.3270 0.069 Uiso 1 1 calc R . .
Li1 Li -0.0831(9) 0.0756(7) 0.0229(7) 0.0354(19) 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'
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'
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
C1 O1 Li1 140.6(4) . . ?
C1 O1 Li1 132.0(4) . 2 ?
Li1 O1 Li1 84.5(4) . 2 ?
C9 O2 C14 118.2(4) . . ?
C17 O3 C22 116.4(5) . . ?
C23 O4 C24 112.6(4) . . ?
C23 O4 Li1 135.2(4) . . ?
C24 O4 Li1 97.4(4) . . ?
C26 O5 C25 113.0(4) . . ?
C26 O5 Li1 132.1(4) . . ?
C25 O5 Li1 112.6(4) . . ?
O1 C1 C6 120.6(4) . . ?
O1 C1 C2 120.2(4) . . ?
C6 C1 C2 119.2(4) . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 C7 123.5(4) . . ?
C1 C2 C7 117.0(4) . . ?
C2 C3 C4 121.7(4) . . ?
C5 C4 C3 119.0(4) . . ?
C4 C5 C6 121.7(4) . . ?
C5 C6 C1 118.9(4) . . ?
C5 C6 C15 121.8(4) . . ?
C1 C6 C15 119.3(4) . . ?
C8 C7 C2 115.3(4) . . ?
C13 C8 C9 116.3(5) . . ?
C13 C8 C7 121.0(5) . . ?
C9 C8 C7 122.8(5) . . ?
C10 C9 C8 123.0(5) . . ?
C10 C9 O2 122.9(5) . . ?
C8 C9 O2 114.2(4) . . ?
C9 C10 C11 119.0(5) . . ?
C12 C11 C10 118.3(5) . . ?
C13 C12 C11 121.3(6) . . ?
C12 C13 C8 122.2(6) . . ?
C16 C15 C6 116.1(4) . . ?
C21 C16 C17 117.1(5) . . ?
C21 C16 C15 121.4(4) . . ?
C17 C16 C15 121.5(4) . . ?
O3 C17 C18 124.5(5) . . ?
O3 C17 C16 114.5(4) . . ?
C18 C17 C16 121.0(5) . . ?
C17 C18 C19 119.7(5) . . ?
C20 C19 C18 122.2(5) . . ?
C19 C20 C21 118.2(6) . . ?
C16 C21 C20 121.8(5) . . ?
O4 C24 C25 111.4(4) . . ?
O4 C24 Li1 50.8(3) . . ?
C25 C24 Li1 81.2(3) . . ?
O5 C25 C24 106.8(4) . . ?
O1 Li1 O1 95.5(4) . 2 ?
O1 Li1 O5 117.0(4) . . ?
O1 Li1 O5 114.8(4) 2 . ?
O1 Li1 O4 138.2(4) . . ?
O1 Li1 O4 110.6(4) 2 . ?
O5 Li1 O4 81.8(3) . . ?
O1 Li1 Li1 48.4(3) . 2 ?
O1 Li1 Li1 47.1(3) 2 2 ?
O5 Li1 Li1 130.4(5) . 2 ?
O4 Li1 Li1 144.3(5) . 2 ?
O1 Li1 C24 163.2(4) . . ?
O1 Li1 C24 101.2(3) 2 . ?
O5 Li1 C24 57.0(3) . . ?
O4 Li1 C24 31.78(18) . . ?
Li1 Li1 C24 148.3(5) 2 . ?
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
O1 C1 1.334(5) . ?
O1 Li1 1.857(9) . ?
O1 Li1 1.897(8) 2 ?
O2 C9 1.399(6) . ?
O2 C14 1.426(6) . ?
O3 C17 1.350(6) . ?
O3 C22 1.435(6) . ?
O4 C23 1.425(6) . ?
O4 C24 1.439(6) . ?
O4 Li1 2.117(9) . ?
O5 C26 1.411(6) . ?
O5 C25 1.419(6) . ?
O5 Li1 2.026(9) . ?
C1 C6 1.409(6) . ?
C1 C2 1.424(6) . ?
C2 C3 1.375(6) . ?
C2 C7 1.515(6) . ?
C3 C4 1.386(6) . ?
C4 C5 1.382(6) . ?
C5 C6 1.398(6) . ?
C6 C15 1.518(6) . ?
C7 C8 1.495(7) . ?
C8 C13 1.393(8) . ?
C8 C9 1.391(7) . ?
C9 C10 1.367(7) . ?
C10 C11 1.423(8) . ?
C11 C12 1.369(8) . ?
C12 C13 1.362(8) . ?
C15 C16 1.512(6) . ?
C16 C21 1.385(7) . ?
C16 C17 1.422(6) . ?
C17 C18 1.373(7) . ?
C18 C19 1.382(7) . ?
C19 C20 1.352(7) . ?
C20 C21 1.420(7) . ?
C24 C25 1.491(7) . ?
C24 Li1 2.709(10) . ?
Li1 O1 1.897(8) 2 ?
Li1 Li1 2.525(17) 2 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139152625
