#------------------------------------------------------------------------------
#$Date: 2025-08-21 12:25:49 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301846 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/72/7007271.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_7007271
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        Et2O
_chemical_formula_moiety         'C48 H54 Li2 O4'
_chemical_formula_sum            'C48 H54 Li2 O4'
_chemical_formula_weight         708.80
_chemical_melting_point          396
_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                77.75(3)
_cell_angle_beta                 89.93(3)
_cell_angle_gamma                68.08(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4436(19)
_cell_length_b                   10.290(2)
_cell_length_c                   11.684(2)
_cell_measurement_temperature    123(2)
_cell_volume                     1025.5(4)
_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 0.956
_diffrn_measured_fraction_theta_max 0.956
_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  0.2431
_diffrn_reflns_av_sigmaI/netI    0.2899
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13933
_diffrn_reflns_theta_full        27.80
_diffrn_reflns_theta_max         27.80
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.9930
_exptl_absorpt_correction_T_min  0.9792
_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    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.776
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.776
_refine_ls_R_factor_all          0.2780
_refine_ls_R_factor_gt           0.0780
_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)+(0.1638P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2971
_reflns_number_gt                1435
_reflns_number_total             4652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602706g.txt
_cod_data_source_block           compound_1
_cod_database_code               7007271
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 0.4967(3) 1.1173(3) -0.0841(2) 0.0401(8) Uani 1 1 d . . .
O2 O 0.6434(4) 1.1086(3) 0.1723(3) 0.0436(9) Uani 1 1 d . . .
C1 C 0.4552(5) 1.2390(5) -0.1674(4) 0.0369(12) Uani 1 1 d . . .
C2 C 0.3067(5) 1.3471(5) -0.1745(4) 0.0359(11) Uani 1 1 d . . .
C3 C 0.2657(5) 1.4703(5) -0.2640(4) 0.0421(12) Uani 1 1 d . . .
H3 H 0.1661 1.5428 -0.2691 0.051 Uiso 1 1 calc R . .
C4 C 0.3655(5) 1.4908(5) -0.3461(4) 0.0419(12) Uani 1 1 d . . .
H4 H 0.3347 1.5763 -0.4065 0.050 Uiso 1 1 calc R . .
C5 C 0.5115(5) 1.3849(5) -0.3393(4) 0.0393(12) Uani 1 1 d . . .
H5 H 0.5803 1.3984 -0.3956 0.047 Uiso 1 1 calc R . .
C6 C 0.5579(5) 1.2594(5) -0.2512(4) 0.0359(11) Uani 1 1 d . . .
C7 C 0.1985(5) 1.3249(5) -0.0855(4) 0.0428(12) Uani 1 1 d . . .
H7A H 0.1951 1.2290 -0.0811 0.051 Uiso 1 1 calc R . .
H7B H 0.0945 1.3976 -0.1136 0.051 Uiso 1 1 calc R . .
C8 C 0.2377(5) 1.3346(5) 0.0370(4) 0.0370(12) Uani 1 1 d . . .
C9 C 0.2024(5) 1.2552(5) 0.1357(4) 0.0448(13) Uani 1 1 d . . .
H9 H 0.1571 1.1893 0.1266 0.054 Uiso 1 1 calc R . .
C10 C 0.2318(6) 1.2696(6) 0.2474(5) 0.0529(14) Uani 1 1 d . . .
H10 H 0.2049 1.2152 0.3138 0.064 Uiso 1 1 calc R . .
C11 C 0.3001(6) 1.3629(6) 0.2626(5) 0.0563(15) Uani 1 1 d . . .
H11 H 0.3208 1.3725 0.3392 0.068 Uiso 1 1 calc R . .
C12 C 0.3380(6) 1.4416(6) 0.1660(5) 0.0563(15) Uani 1 1 d . . .
H12 H 0.3849 1.5062 0.1757 0.068 Uiso 1 1 calc R . .
C13 C 0.3078(6) 1.4270(5) 0.0540(4) 0.0488(14) Uani 1 1 d . . .
H13 H 0.3356 1.4812 -0.0122 0.059 Uiso 1 1 calc R . .
C14 C 0.7158(5) 1.1423(5) -0.2422(4) 0.0420(12) Uani 1 1 d . . .
H14A H 0.7603 1.1139 -0.1597 0.050 Uiso 1 1 calc R . .
H14B H 0.7050 1.0571 -0.2615 0.050 Uiso 1 1 calc R . .
C15 C 0.8264(5) 1.1832(5) -0.3210(4) 0.0357(11) Uani 1 1 d . . .
C16 C 0.8505(5) 1.1488(5) -0.4296(4) 0.0404(12) Uani 1 1 d . . .
H16 H 0.8024 1.0915 -0.4535 0.049 Uiso 1 1 calc R . .
C17 C 0.9444(5) 1.1973(5) -0.5043(4) 0.0463(13) Uani 1 1 d . . .
H17 H 0.9595 1.1728 -0.5786 0.056 Uiso 1 1 calc R . .
C18 C 1.0145(5) 1.2793(5) -0.4719(4) 0.0456(13) Uani 1 1 d . . .
H18 H 1.0759 1.3142 -0.5244 0.055 Uiso 1 1 calc R . .
C19 C 0.9966(5) 1.3118(5) -0.3626(4) 0.0469(13) Uani 1 1 d . . .
H19 H 1.0483 1.3662 -0.3384 0.056 Uiso 1 1 calc R . .
C20 C 0.9020(5) 1.2642(5) -0.2884(4) 0.0425(12) Uani 1 1 d . . .
H20 H 0.8889 1.2875 -0.2137 0.051 Uiso 1 1 calc R . .
C21 C 0.6874(6) 1.0696(5) 0.2960(4) 0.0484(14) Uani 1 1 d . . .
H21A H 0.6551 1.1569 0.3282 0.058 Uiso 1 1 calc R . .
H21B H 0.8002 1.0204 0.3105 0.058 Uiso 1 1 calc R . .
C22 C 0.6119(5) 0.9710(5) 0.3550(4) 0.0504(14) Uani 1 1 d . . .
H22A H 0.5005 1.0196 0.3387 0.076 Uiso 1 1 calc R . .
H22B H 0.6385 0.9458 0.4401 0.076 Uiso 1 1 calc R . .
H22C H 0.6475 0.8833 0.3248 0.076 Uiso 1 1 calc R . .
C23 C 0.7040(6) 1.2089(6) 0.1084(5) 0.0527(14) Uani 1 1 d . . .
H23A H 0.6912 1.2846 0.1521 0.063 Uiso 1 1 calc R . .
H23B H 0.6444 1.2559 0.0311 0.063 Uiso 1 1 calc R . .
C24 C 0.8688(6) 1.1398(7) 0.0898(5) 0.083(2) Uani 1 1 d . . .
H24A H 0.9302 1.1050 0.1657 0.124 Uiso 1 1 calc R . .
H24B H 0.9010 1.2103 0.0382 0.124 Uiso 1 1 calc R . .
H24C H 0.8839 1.0587 0.0534 0.124 Uiso 1 1 calc R . .
Li1 Li 0.5094(9) 1.0608(9) 0.0782(7) 0.045(2) 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 138.6(4) . . ?
C1 O1 Li1 133.7(4) . 2_675 ?
Li1 O1 Li1 83.7(4) . 2_675 ?
C21 O2 C23 112.8(4) . . ?
C21 O2 Li1 132.2(3) . . ?
C23 O2 Li1 114.8(3) . . ?
O1 C1 C6 120.3(4) . . ?
O1 C1 C2 120.3(4) . . ?
C6 C1 C2 119.4(4) . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 C7 122.0(4) . . ?
C1 C2 C7 119.2(4) . . ?
C4 C3 C2 122.0(4) . . ?
C3 C4 C5 119.3(4) . . ?
C4 C5 C6 120.9(4) . . ?
C5 C6 C1 119.6(4) . . ?
C5 C6 C14 121.9(4) . . ?
C1 C6 C14 118.5(4) . . ?
C2 C7 C8 115.3(4) . . ?
C9 C8 C13 117.6(4) . . ?
C9 C8 C7 121.6(4) . . ?
C13 C8 C7 120.8(4) . . ?
C10 C9 C8 121.4(5) . . ?
C11 C10 C9 120.2(5) . . ?
C10 C11 C12 119.4(5) . . ?
C11 C12 C13 120.1(5) . . ?
C12 C13 C8 121.2(5) . . ?
C15 C14 C6 114.9(4) . . ?
C16 C15 C20 117.6(4) . . ?
C16 C15 C14 122.1(4) . . ?
C20 C15 C14 120.2(4) . . ?
C15 C16 C17 120.8(5) . . ?
C18 C17 C16 120.6(5) . . ?
C17 C18 C19 120.0(5) . . ?
C18 C19 C20 119.3(5) . . ?
C19 C20 C15 121.6(5) . . ?
O2 C21 C22 108.6(4) . . ?
O2 C23 C24 112.9(4) . . ?
O1 Li1 O1 96.3(4) . 2_675 ?
O1 Li1 O2 119.5(4) . . ?
O1 Li1 O2 128.0(4) 2_675 . ?
O1 Li1 Li1 48.0(3) . 2_675 ?
O1 Li1 Li1 48.3(3) 2_675 2_675 ?
O2 Li1 Li1 146.1(6) . 2_675 ?
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 1.337(5) . ?
O1 Li1 1.851(8) . ?
O1 Li1 1.842(9) 2_675 ?
O2 C21 1.434(5) . ?
O2 C23 1.436(5) . ?
O2 Li1 1.935(9) . ?
C1 C6 1.417(6) . ?
C1 C2 1.416(6) . ?
C2 C3 1.387(6) . ?
C2 C7 1.500(6) . ?
C3 C4 1.383(6) . ?
C4 C5 1.392(6) . ?
C5 C6 1.390(6) . ?
C6 C14 1.514(6) . ?
C7 C8 1.511(6) . ?
C8 C9 1.382(6) . ?
C8 C13 1.390(6) . ?
C9 C10 1.385(7) . ?
C10 C11 1.379(7) . ?
C11 C12 1.373(7) . ?
C12 C13 1.391(7) . ?
C14 C15 1.509(6) . ?
C15 C16 1.385(6) . ?
C15 C20 1.389(6) . ?
C16 C17 1.393(6) . ?
C17 C18 1.359(7) . ?
C18 C19 1.382(7) . ?
C19 C20 1.391(6) . ?
C21 C22 1.502(6) . ?
C23 C24 1.488(7) . ?
Li1 O1 1.842(9) 2_675 ?
Li1 Li1 2.465(17) 2_675 ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139152622
