Synthesis and structures of crystalline Li, Al and Sn(ii) 1-azaallyls and β-diketiminates derived from [Li{μ,η3-N(SiMe3)C(Ad)C(H)SiMe3}]2 (Ad = 1-adamantyl)
Bourget-Merle, Laurence; Hitchcock, Peter B.; Lappert, Michael F.; Merle, Philippe G.; Dalton Transactions  (2008) 3493–3501; doi:10.1039/b718728a

data_7003695
_publ_section_title
;
 Synthesis and structures of crystalline Li, Al and Sn(ii) 1-azaallyls
 and \b-diketiminates derived from [Li{\m,\h3-N(SiMe3)C(Ad)C(H)SiMe3}]2
 (Ad = 1-adamantyl)
;
_journal_issue                   26
_journal_name_full               'Dalton Transactions'
_journal_page_first              3493
_journal_page_last               3501
_journal_paper_doi               10.1039/b718728a
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H68 N2 Si4 Sn'
_chemical_formula_sum            'C36 H68 N2 Si4 Sn'
_chemical_formula_weight         759.97
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/cifdics/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1
_audit_creation_date             2000-07-28T16:44:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1969(3)
_cell_length_b                   23.3707(5)
_cell_length_c                   22.0743(3)
_cell_measurement_reflns_used    25849
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     8355.8(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38603
_diffrn_reflns_theta_full        27.86
_diffrn_reflns_theta_max         27.86
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0326
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+5.5835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.073
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                7747
_reflns_number_total             9857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718728a.txt
_cod_data_source_block           (7)-jul2900
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7003695