Synthesis, structure, and computational studies of the tetrameric magnesium imides [2,4,6-Cl3C6H2NMg.S]4 (S=1,4-dioxane and tetrahydrofuran).
Rood, Jeffrey A.; Noll, Bruce C.; Henderson, Kenneth W.; Inorganic chemistry 46 (2007) 7259–7261; doi:10.1021/ic701104s

data_4338904
_publ_section_title
;
 Synthesis, structure, and computational studies of the tetrameric
 magnesium imides [2,4,6-Cl3C6H2NMg.S]4 (S=1,4-dioxane and
 tetrahydrofuran).
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7259
_journal_page_last               7261
_journal_paper_doi               10.1021/ic701104s
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C40 H40 Cl12 Mg4 N4 O4, C7 H8'
_chemical_formula_sum            'C47 H48 Cl12 Mg4 N4 O4'
_chemical_formula_weight         1255.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.4380(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3452(2)
_cell_length_b                   12.8441(2)
_cell_length_c                   25.5481(4)
_cell_measurement_reflns_used    8250
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.8837
_cell_measurement_theta_min      3.1042
_cell_volume                     5347.47(14)
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004; Sheldrick, 2003)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)/enCIFer (CCDC, 2004)'
_computing_structure_refinement  'XL (Sheldrick, 2001)'
_computing_structure_solution    'XS (Sheldrick, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART Apex CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            38948
_diffrn_reflns_theta_full        66.49
_diffrn_reflns_theta_max         66.49
_diffrn_reflns_theta_min         3.10
_diffrn_source_type              'Siemens KFFCU2K-90'
_exptl_absorpt_coefficient_mu    6.544
_exptl_absorpt_correction_T_max  0.20
_exptl_absorpt_correction_T_min  0.17
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Sheldrick, G.M. (2004) SADABS, University of G\"ottingen, Germany.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.267
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.245
_refine_diff_density_max         1.171
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         8869
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+5.7487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                7400
_reflns_number_total             8869
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701104s-file002.cif
_cod_data_source_block           compound_5
_cod_original_cell_volume        5347.47(13)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4338904