Dis-assembling lithium amide ladder structures: new insight through the structure of [{[PhCH2N(H)Li]2·thf}∞ ], a polymer of (NLi)2 planar rings connected by thf-bridged (NLi)2 butterfly junctions
Clegg, William; Liddle, Stephen T.; Mulvey, Robert E.; Robertson, Alan; Chemical Communications  (1999) 511–; doi:10.1039/a900392d

data_7110452
_publ_section_title
;
 Dis-assembling lithium amide ladder structures: new insight through the
 structure of [{[PhCH2N(H)Li]2&#x00B7;thf}\\infty ], a polymer of (NLi)2
 planar rings connected by thf-bridged (NLi)2 butterfly junctions
;
_journal_issue                   6
_journal_name_full               'Chemical Communications'
_journal_page_first              511
_journal_paper_doi               10.1039/a900392d
_journal_year                    1999
_chemical_formula_sum            'C18 H24 Li2 N2 O'
_chemical_formula_weight         298.27
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.617(5)
_cell_length_b                   10.047(2)
_cell_length_c                   7.594(2)
_cell_measurement_reflns_used    53
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      18.33
_cell_volume                     1725.6(7)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_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 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Stoe-Siemens diffractometer'
_diffrn_measurement_method       '\w/\q scans with on-line profile fitting'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            4028
_diffrn_reflns_theta_full        67.58
_diffrn_reflns_theta_max         67.58
_diffrn_reflns_theta_min         7.35
_diffrn_standards_decay_%        6.6
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.202
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1528
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0509
_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/[\s^2^(Fo^2^)+(0.0748P)^2^+0.4541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                1151
_reflns_number_total             1528
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900392dsup1.cif
_cod_data_source_block           rem181
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7110452