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_4320522
_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            'C12 H24 I2 Mg O3'
_chemical_formula_weight         494.42
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 112.67(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.234(4)
_cell_length_b                   12.600(4)
_cell_length_c                   12.395(3)
_cell_measurement_reflns_used    55
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      16.36
_cell_measurement_theta_min      4.70
_cell_volume                     1763.1(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2441
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.602
_exptl_absorpt_correction_T_max  0.7916
_exptl_absorpt_correction_T_min  0.3385
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.54
_exptl_crystal_size_min          0.38
_refine_diff_density_max         2.548
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.048
_refine_ls_goodness_of_fit_obs   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1956
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_restrained_S_obs      1.069
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_obs          0.0508
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+7.2742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1538
_refine_ls_wR_factor_obs         0.1340
_reflns_number_observed          1743
_reflns_number_total             1962
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010513m_3.cif
_cod_data_source_block           rw963a_COMPOUND4
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+7.2742P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0908P)^2^+7.2742P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1763.0(9)
_cod_database_code               4320522