A new approach to lithium–heavier alkali metal interchange reactions: synthesis of a tetralithium pentasodium mixed alkoxide–amide dome-shaped cage compound with an encapsulated hydroxide molecule †
Kennedy, Alan R.; MacLellan, Jonathan G.; Mulvey, Robert E.; Robertson, Alan; Journal of the Chemical Society, Dalton Transactions  (2000) 4112–; doi:10.1039/b006990f

data_7010211
_publ_section_title
;
 A new approach to lithium--heavier alkali metal interchange reactions:
 synthesis of a tetralithium pentasodium mixed alkoxide--amide
 dome-shaped cage compound with an encapsulated hydroxide
 molecule&#x200A;&#x2020;
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4112
_journal_paper_doi               10.1039/b006990f
_journal_year                    2000
_chemical_formula_sum            'C64 H89 Li4 N8 Na5 O5'
_chemical_formula_weight         1193.14
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.87(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.808(9)
_cell_length_b                   9.246(4)
_cell_length_c                   29.477(9)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      12.17
_cell_measurement_theta_min      5.98
_cell_volume                     7065(5)
_computing_cell_refinement       ' " '
_computing_data_collection       'MSC Diff. Control'
_computing_data_reduction        texsan
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.466
_diffrn_measured_fraction_theta_max 0.466
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            5683
_diffrn_reflns_theta_full        24.02
_diffrn_reflns_theta_max         24.02
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        1.986
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9857
_exptl_absorpt_correction_T_min  0.9401
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colourless
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1286
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+4.9431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2061
_refine_ls_wR_factor_ref         0.2335
_reflns_number_gt                3608
_reflns_number_total             5559
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006990f.txt
_cod_data_source_block           jon
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1157P)^2^+4.9431P] 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^)+(0.1157P)^2^+4.9431P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7065(4)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7010211