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_4320520
_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            'C20 H40 I4 Mg O5'
_chemical_formula_weight         892.43
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.592(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.631(3)
_cell_length_b                   11.027(2)
_cell_length_c                   16.174(4)
_cell_measurement_reflns_used    56
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.01
_cell_measurement_theta_min      4.72
_cell_volume                     2946.5(11)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0403
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            3237
_diffrn_reflns_theta_full        26.51
_diffrn_reflns_theta_max         26.51
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        1.6
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.276
_exptl_absorpt_correction_T_max  0.3242
_exptl_absorpt_correction_T_min  0.1905
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.981
_refine_diff_density_min         -1.357
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0542P)^2^+10.6623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1043
_reflns_number_gt                2611
_reflns_number_total             3048
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010513m_1.cif
_cod_data_source_block           rw114c_COMPOUND6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        2946.6(10)
_cod_database_code               4320520