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_4338903
_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 O8, 3(C4 H8 O2)'
_chemical_formula_sum            'C52 H64 Cl12 Mg4 N4 O14'
_chemical_formula_weight         1491.71
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.57(3)
_cell_angle_beta                 81.47(3)
_cell_angle_gamma                73.71(3)
_cell_formula_units_Z            2
_cell_length_a                   13.922(3)
_cell_length_b                   15.111(3)
_cell_length_c                   17.506(4)
_cell_measurement_reflns_used    11643
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2937
_cell_measurement_theta_min      1.4713
_cell_volume                     3264.0(15)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            88818
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.26
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    0.611
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.83
_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    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.216
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.225
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         13330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/su_max          0.041
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+8.4457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1473
_reflns_number_gt                12350
_reflns_number_total             13330
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701104s-file002.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3264.0(11)
_cod_database_code               4338903