Synthesis and Characterization of an Unsolvated Dimeric Diarylmagnesium Compound and Its Magnesium Iodide Byproducts
Rudolf J. Wehmschulte; Brendan Twamley; Masood A. Khan; Inorganic Chemistry 40 (2001) 6004–6008; doi:10.1021/ic010513m

data_4320523
_publ_contact_author_address
;       Department of Chemistry and Biochemistry
       University of Oklahoma
       620 Parrington Oval, Room 208
       Norman, OK 73019
;
_publ_contact_author_email       rjwehmschulte@ou.edu
_publ_contact_author_fax         '405 325 6111'
_publ_contact_author_name        'Rudolf J. Wehmschulte'
_publ_contact_author_phone       '405 325 2388'
_publ_section_title
;
 Synthesis and Characterization of an Unsolvated Dimeric Diarylmagnesium
 Compound and Its Magnesium Iodide Byproducts
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6004
_journal_page_last               6008
_journal_paper_doi               10.1021/ic010513m
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H48 I2 Mg O6'
_chemical_formula_weight         710.73
_space_group_IT_number           201
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-P 2ab 2bc 3'
_symmetry_space_group_name_H-M   'P n -3 :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.279(2)
_cell_length_b                   14.279(2)
_cell_length_c                   14.279(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      4.96
_cell_volume                     2911.3(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            1601
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.02
_diffrn_standards_decay_%        1.4
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.216
_exptl_absorpt_correction_T_max  0.5374
_exptl_absorpt_correction_T_min  0.4563
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.622
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.595
_refine_diff_density_min         -1.061
_refine_diff_density_rms         0.258
_refine_ls_extinction_coef       0.0017(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         858
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.1846
_refine_ls_R_factor_gt           0.1244
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0797P)^2^+264.5737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2950
_refine_ls_wR_factor_ref         0.3322
_reflns_number_gt                460
_reflns_number_total             858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010513m_4.cif
_cod_data_source_block           rw052b_COMPOUND5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2911.3(8)
_cod_original_sg_symbol_H-M      'P n -3'
_cod_database_code               4320523