Unprecedented CpLi Ammoniacates
Michel, Reent; Herbst-Irmer, Regine; Stalke, Dietmar; Organometallics 29 (2010) 6169–; doi:10.1021/om100831v

data_4067102
_publ_contact_author             'Prof. Dr. D. Stalke'
_publ_section_title
;
 Unprecedented CpLi Ammoniacates
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6169
_journal_paper_doi               10.1021/om100831v
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C5 H20 Li N5'
_chemical_formula_weight         157.20
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            8
_cell_length_a                   24.603(4)
_cell_length_b                   6.886(2)
_cell_length_c                   12.638(2)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.925
_cell_measurement_theta_min      3.072
_cell_volume                     2141.1(8)
_computing_cell_refinement       'SAINT V7.46A'
_computing_data_collection       'APEX2 v2009.3-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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 Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            41275
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Sheldrick 2008'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.975
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.8
_refine_diff_density_max         0.376
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3398
_refine_ls_number_restraints     1147
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0599
_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^)+(0.1151P)^2^+1.1708P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2015
_reflns_number_gt                3147
_reflns_number_total             3398
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100831v_si_004.cif
_cod_data_source_block           pna21
_cod_original_sg_symbol_H-M      Pna2(1)
_cod_database_code               4067102