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_4346509
_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         'C30 H86 Br N7 Na4 Si6'
_chemical_formula_sum            'C30 H86 Br N7 Na4 Si6'
_chemical_formula_weight         885.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.652(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.0031(2)
_cell_length_b                   14.6586(2)
_cell_length_c                   20.7632(3)
_cell_measurement_reflns_used    15447
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      72.9260
_cell_measurement_theta_min      5.2020
_cell_volume                     2734.61(8)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31873
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         69.991
_diffrn_reflns_theta_min         3.015
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       needle
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 3596 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.028(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9420
_refine_ls_number_restraints     152
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+2.8462P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1296
_refine_ls_wR_factor_ref         0.1418
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.820
_reflns_Friedel_fraction_max     0.820
_reflns_number_gt                8438
_reflns_number_total             9420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01584_si_002.cif
_cod_data_source_block           amao330smart
_cod_original_sg_symbol_H-M      'P n'
_cod_database_code               4346509
_shelxl_version_number           2013-4
_shelx_res_checksum              70637
_shelx_hkl_checksum              67289