Synthetic and Structural Studies of Mixed Sodium Bis(trimethylsilyl)amide/Sodium Halide Aggregates in the Presence of η(2)-N,N-, η(3)-N,N,N/N,O,N-, and η(4)-N,N,N,N-Donor Ligands.
Ojeda-Amador, Ana I; Martínez-Martínez, Antonio J; Kennedy, Alan R.; O'Hara, Charles T; Inorganic chemistry 54 (2015) 9833–9844; doi:10.1021/acs.inorgchem.5b01584

data_4346503
_publ_section_title
;
 Synthetic and Structural Studies of Mixed Sodium
 Bis(trimethylsilyl)amide/Sodium Halide Aggregates in the Presence of
 \h(2)-N,N-, \h(3)-N,N,N/N,O,N-, and \h(4)-N,N,N,N-Donor Ligands.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9833
_journal_page_last               9844
_journal_paper_doi               10.1021/acs.inorgchem.5b01584
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C42 H120 Cl1 N9 Na6 Si10'
_chemical_formula_sum            'C42 H120 Cl N9 Na6 Si10'
_chemical_formula_weight         1205.76
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_atom_sites_solution_primary     direc
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.097(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7203(3)
_cell_length_b                   20.5494(3)
_cell_length_c                   14.5519(2)
_cell_measurement_reflns_used    23951
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      30.1566
_cell_measurement_theta_min      3.0156
_cell_volume                     3853.01(12)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_publication_material  'SHELXL-2013 '
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0377
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47741
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.876
_diffrn_reflns_theta_min         3.022
_exptl_absorpt_coefficient_mu    0.270
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92630
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_description       block
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.174
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 7091 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         18023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.1068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0761
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                16195
_reflns_number_total             18023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01584_si_002.cif
_cod_data_source_block           amao131
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C42 H120 Cl1 N9 Na6 Si10'
_cod_database_code               4346503
_shelxl_version_number           2013-4
_shelx_res_checksum              997
_shelx_hkl_checksum              80741