Synthesis of the mixed lithium‒potassium‒(bis)magnesium N-metallated/N, C-dimetallated amide [Li2K2Mg4{But(Me3Si)N}4{But[Me2(H2C)Si]N}4]: an inverse crown molecule with an atomless cavity
Forbes, Glenn C.; Kenley, Fiona R.; Kennedy, Alan R.; Mulvey, Robert E.; O'Hara, Charles T.; Parkinson, John A.; Chemical Communications (Cambridge, United Kingdom)  (2003) 1140–1141; doi:10.1039/b301374j

data_7113612
_publ_section_title
;
 Synthesis of the mixed lithium--potassium--(bis)magnesium N-metallated/N,
 C-dimetallated amide [Li2K2Mg4{But(Me3Si)N}4{But[Me2(H2C)Si]N}4]: an
 inverse crown molecule with an atomless cavity
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_journal_coden_ASTM              CHCOFS
_journal_issue                   10
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              1140
_journal_page_last               1141
_journal_paper_doi               10.1039/b301374j
_journal_year                    2003
_chemical_formula_sum            'C62 H154 K2 Li2 Mg4 N8 Si8'
_chemical_formula_weight         1425.97
_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                 106.135(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.5490(2)
_cell_length_b                   14.6937(1)
_cell_length_c                   43.9600(3)
_cell_measurement_reflns_used    23129
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.91
_cell_volume                     18334.9(3)
_computing_data_collection       'Collect and Denzo'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Shelxls-97
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'omega and phi 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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            33036
_diffrn_reflns_theta_full        26.85
_diffrn_reflns_theta_max         26.85
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'fragment from large prism'
_exptl_crystal_F_000             6288
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.653
_refine_diff_density_min         -0.589
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         19142
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+39.9099P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                15434
_reflns_number_total             19142
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7103648
_cod_data_source_file            b301374j.txt
_cod_data_source_block           grem82
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        18334.9(2)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113612