Pentanuclear asymmetrical ladder structure of the 1,4-dimethylpiperazine solvate of lithium anilide and its implication for the unknown structure of amorphous lithium anilide
Clegg, William; Liddle, Stephen T.; Mulvey, Robert E.; Robertson, Alan; Chemical Communications  (2000) 223–; doi:10.1039/a909754f

data_7110817
_publ_section_title
;
 Pentanuclear asymmetrical ladder structure of the 1,4-dimethylpiperazine
 solvate of lithium anilide and its implication for the unknown structure
 of amorphous lithium anilide
;
_journal_issue                   3
_journal_name_full               'Chemical Communications'
_journal_page_first              223
_journal_paper_doi               10.1039/a909754f
_journal_year                    2000
_chemical_formula_sum            'C59 H81 Li5 N10'
_chemical_formula_weight         965.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                64.592(3)
_cell_angle_beta                 80.095(4)
_cell_angle_gamma                85.225(4)
_cell_formula_units_Z            2
_cell_length_a                   11.2049(16)
_cell_length_b                   16.726(3)
_cell_length_c                   17.152(3)
_cell_measurement_reflns_used    7180
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.10
_cell_volume                     2860.1(8)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0855
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17166
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0048(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     683
_refine_ls_number_reflns         9732
_refine_ls_number_restraints     161
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1501
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1372P)^2^+0.7073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2192
_refine_ls_wR_factor_ref         0.2625
_reflns_number_gt                5443
_reflns_number_total             9732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            a909754fsup1.cif
_cod_data_source_block           rem200
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110817