The low-temperature structure of diethyl ether magnesium oxybromide
Vitze, Hannes; Lerner, Hans-Wolfram; Bolte, Michael; Acta Crystallographica Section E 67 (2011) m1614–; doi:10.1107/S1600536811043820

data_2232153
_publ_section_title
;
 The low-temperature structure of diethyl ether magnesium oxybromide
;
_journal_coeditor_code           BH2385
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1614
_journal_paper_doi               10.1107/S1600536811043820
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Mg4 Br6 O (C4 H10 O)4]'
_chemical_formula_moiety         'C16 H40 Br6 Mg4 O5'
_chemical_formula_sum            'C16 H40 Br6 Mg4 O5'
_chemical_formula_weight         889.18
_chemical_name_systematic
;
hexa-\m~2~-bromido-\m~4~-oxido-tetrakis[(diethyl ether)magnesium]
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.4630(13)
_cell_length_b                   10.4630(13)
_cell_length_c                   15.276(2)
_cell_measurement_reflns_used    3746
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.6
_cell_measurement_theta_min      3.8
_cell_volume                     1672.3(4)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3746
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         3.83
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.299
_exptl_absorpt_correction_T_max  0.2685
_exptl_absorpt_correction_T_min  0.1691
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.561
_refine_ls_abs_structure_details 'Flack (1983), with 689 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_coef       0.0036(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     73
_refine_ls_number_reflns         1479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.2840P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                1455
_reflns_number_total             1479
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2385.cif
_cod_data_source_block           I
_cod_database_code               2232153
_cod_database_fobs_code          2232153