Cation-induced structural variations in the alkali metal derivatives of 2-trimethylsilylaminopyridine: synthesis and X-ray structures of complexes for all five metals Li–Cs with 12-crown-4 †
Liddle, Stephen T.; Clegg, William; Journal of the Chemical Society, Dalton Transactions  (2001) 402–; doi:10.1039/b008852h

data_7010423
_publ_section_title
;
 Cation-induced structural variations in the alkali metal derivatives
 of 2-trimethylsilylaminopyridine: synthesis and X-ray structures of
 complexes for all five metals Li--Cs with 12-crown-4&#x200A;&#x2020;
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              402
_journal_paper_doi               10.1039/b008852h
_journal_year                    2001
_chemical_formula_sum            'C46 H74 K2 N4 O8 Si2'
_chemical_formula_weight         945.47
_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                71.065(2)
_cell_angle_beta                 88.749(2)
_cell_angle_gamma                72.796(2)
_cell_formula_units_Z            1
_cell_length_a                   10.5289(7)
_cell_length_b                   11.6308(8)
_cell_length_c                   11.9792(8)
_cell_measurement_reflns_used    9231
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.35
_cell_volume                     1321.03(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.893
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11488
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.275
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.590
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.188
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.52
_refine_diff_density_max         1.123
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.002(2)
_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   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         6034
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1547
_reflns_number_gt                4086
_reflns_number_total             6034
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b008852h.txt
_cod_data_source_block           4
_cod_original_cell_volume        1321.03(15)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7010423