Mixed Crystalline Lithium Organics and Interconversion in Solution
Pöppler, Ann-Christin; Meinholz, Margret M.; Faßhuber, Hannes; Lange, Adam; John, Michael; Stalke, Dietmar; Organometallics 31 (2012) 42–; doi:10.1021/om2010639

data_4068071
_publ_section_title
;
 Mixed Crystalline Lithium Organics and Interconversion in Solution
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              42
_journal_paper_doi               10.1021/om2010639
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C16 H36 Li4, 4(C32 H40 Li4 N4)'
_chemical_formula_sum            'C144 H196 Li20 N16'
_chemical_formula_weight         2289.97
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_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            2
_cell_length_a                   27.993(4)
_cell_length_b                   27.993(4)
_cell_length_c                   8.8744(12)
_cell_measurement_reflns_used    7911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.2635
_cell_measurement_theta_min      2.3005
_cell_volume                     6954.1(17)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'Apex v2010.7-0'
_computing_data_reduction        'SAINT V7.68A'
_computing_structure_refinement  'SHELXL in SHELXTL 2008/4 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS in SHELXTL 2008/4 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC quazar mirror optics'
_diffrn_radiation_source         'INCOATEC Mo micro source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            40145
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.7689
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.094
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.183
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         3964
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0428P)^2^+3.3274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0950
_reflns_number_gt                3512
_reflns_number_total             3964
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2010639_si_002.cif
_cod_data_source_block           sad
_cod_original_cell_volume        6954.3(16)
_cod_original_sg_symbol_H-M      I-4
_cod_database_code               4068071