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_4346504
_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 Br N9 Na6 Si10'
_chemical_formula_sum            'C42 H120 Br N9 Na6 Si10'
_chemical_formula_weight         1250.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 110.422(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.7374(3)
_cell_length_b                   20.6050(3)
_cell_length_c                   14.5508(3)
_cell_measurement_reflns_used    14778
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.3330
_cell_measurement_theta_min      3.1440
_cell_volume                     3859.87(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_publication_material  'SHELXL-2013 '
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40805
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.411
_diffrn_reflns_theta_min         2.645
_exptl_absorpt_coefficient_mu    0.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84171
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.076
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 5910 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         19344
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0351P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.779
_reflns_Friedel_fraction_full    0.943
_reflns_Friedel_fraction_max     0.744
_reflns_number_gt                15755
_reflns_number_total             19344
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01584_si_002.cif
_cod_data_source_block           amao150
_cod_original_cell_volume        3859.86(15)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4346504
_shelxl_version_number           2013-4
_shelx_res_checksum              95115
_shelx_hkl_checksum              23003