Hydride Encapsulation by a Molecular Main-Group-Metal Cluster: Single-Crystal Neutron Diffraction Structure of [{Ph(2-C5H4N)N}6HLi8]+
Boss, Sally R.; Cole, Jacqueline M.; Haigh, Robert; Snaith, Ronald; Wheatley, Andrew E. H.; McIntyre, Garry J.; Raithby, Paul R.; Organometallics 23 (2004) 4527–; doi:10.1021/om049661l

data_4083987
_publ_section_title
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 Hydride Encapsulation by a Molecular Main-Group-Metal Cluster:&#x00A0;
 Single-Crystal Neutron Diffraction Structure of [{Ph(2-C5H4N)N}6HLi8]+
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_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4527
_journal_paper_doi               10.1021/om049661l
_journal_volume                  23
_journal_year                    2004
_chemical_formula_sum            'C86 H103 Al2 Li9 N12'
_chemical_formula_weight         1420.00
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     'previous X-ray structure model'
_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            4
_cell_length_a                   19.546(4)
_cell_length_b                   16.0980(10)
_cell_length_c                   26.168(6)
_cell_measurement_temperature    1.5(5)
_cell_volume                     8234(3)
_computing_cell_refinement       'LAUEGEN (Campbell, 1995 and 1998)'
_computing_data_collection       'local program'
_computing_data_reduction        'Integrate+ (Wilkinson et al, 1988)'
_computing_molecular_graphics    'SHEXLTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      1.5(5)
_diffrn_measured_fraction_theta_full 0.801
_diffrn_measured_fraction_theta_max 0.801
_diffrn_measurement_device_type
'Very Intense Vertical Axis Laue Diffractometer (VIVALDI)''
_diffrn_measurement_method       'Laue diffraction'
_diffrn_radiation_monochromator  'none (polychromatic)'
_diffrn_radiation_source
'Institut Laue Langevin (ILL), Grenoble, France'
_diffrn_radiation_type           'neutrons (polychromatic)'
_diffrn_radiation_wavelength     '1.1-2.5 used for scaling''
_diffrn_reflns_av_R_equivalents  0.2246
_diffrn_reflns_av_sigmaI/netI    0.1027
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33746
_diffrn_reflns_theta_full        31.72
_diffrn_reflns_theta_max         31.72
_diffrn_reflns_theta_min         3.50
_exptl_absorpt_coefficient_mu    0.115*lambda+0.101
_exptl_absorpt_correction_T_max  0.730
_exptl_absorpt_correction_T_min  0.412
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trapezoid block'
_exptl_crystal_F_000             1154
_exptl_crystal_size_max          2.50
_exptl_crystal_size_mid          2.00
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.940
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     684
_refine_ls_number_reflns         3024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.940
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0972
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                2547
_reflns_number_total             3024
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            compound1.cif
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

'_cell_measurement_temperature' value '1.5(0.5)' was changed to
'1.5(5)' - precision was estimated.

'_diffrn_ambient_temperature'
value '1.5(0.5)' was changed to '1.5(5)' - precision was estimated.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               4083987