Microsolvation and 13C-Li NMR Coupling
Rudolf Knorr; Thomas Menke; Kathrin Ferchland; Johann Mehlstäubl; David S. Stephenson; Journal of the American Chemical Society 130 (2008) 14179–14188; doi:10.1021/ja8026828

data_4108531
_publ_section_title
;
 Microsolvation and 13C-Li NMR Coupling
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14179
_journal_page_last               14188
_journal_paper_doi               10.1021/ja8026828
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C55 H66 Li2 O2'
_chemical_formula_weight         772.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 104.01(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.465(4)
_cell_length_b                   9.769(3)
_cell_length_c                   25.461(6)
_cell_measurement_temperature    173
_cell_volume                     4697(2)
_computing_cell_refinement       'XSCANS (Ver. 2.00)'
_computing_data_collection       'XSCANS (Ver. 2.00)'
_computing_data_reduction        'XSCANS (Ver. 2.00)'
_computing_molecular_graphics    'XP (SHELXTL-Plus)'
_computing_publication_material  'SHELXL (Sheldrick 1993)'
_computing_structure_refinement  'SHELXL (Sheldrick 1993)'
_computing_structure_solution    'XS (Siemens)'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       P4
_diffrn_measurement_method       \w
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.0770
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            5752
_diffrn_reflns_theta_max         23.00
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.063
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.016
_refine_ls_goodness_of_fit_obs   1.090
_refine_ls_hydrogen_treatment    'riding model, fixed isotropic U'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_restrained_S_obs      1.090
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_obs          0.0548
_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/[\s^2^(Fo^2^)+(0.0635P)^2^+2.5397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1529
_refine_ls_wR_factor_obs         0.1187
_reflns_number_observed          1816
_reflns_number_total             3212
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja8026828_si_003.cif
_cod_data_source_block           knorr3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+2.5397P] 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^)+(0.0635P)^2^+2.5397P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_hydrogens' value 'geometrically' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        4697.5(21)
_cod_database_code               4108531