Formation of [M(15-crown-5)2]2[Li(NHPy)3] (M = K or Cs): the first structurally authenticated examples of a monomeric lithium species coordinated by three amide anions
Liddle, Stephen T.; Clegg, William; Journal of the Chemical Society, Dalton Transactions  (2001) 3549–; doi:10.1039/b109903p

data_7702758
_publ_section_title
;
 Formation of [M(15-crown-5)2]2[Li(NHPy)3] (M = K or Cs): the first
 structurally authenticated examples of a monomeric lithium species
 coordinated by three amide anions
;
_journal_issue                   24
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3549
_journal_paper_doi               10.1039/b109903p
_journal_year                    2001
_chemical_formula_sum            'C55 H95 Cs2 Li N6 O20'
_chemical_formula_weight         1433.13
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                77.781(2)
_cell_angle_beta                 71.818(2)
_cell_angle_gamma                68.921(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2706(9)
_cell_length_b                   14.6824(9)
_cell_length_c                   18.2599(11)
_cell_measurement_reflns_used    13524
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      28.47
_cell_measurement_theta_min      2.36
_cell_volume                     3370.3(4)
_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      220(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.891
_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  0.0237
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29613
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.66
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.153
_exptl_absorpt_correction_T_max  0.4762
_exptl_absorpt_correction_T_min  0.3478
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.510
_refine_diff_density_min         -0.680
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.884
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     766
_refine_ls_number_reflns         15450
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          3.404
_refine_ls_shift/su_mean         0.663
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1333P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1820
_refine_ls_wR_factor_ref         0.2108
_reflns_number_gt                7548
_reflns_number_total             15450
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b109903p.txt
_cod_data_source_block           stl57
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7702758