Structural and EPR characterisation of single electron and alkyl transfer products from reaction of dimethyl magnesium with bulky alpha-diimine ligands.
Bailey, Philip J.; Coxall, Robert A.; Dick, Caroline M.; Fabre, Sylvie; Parsons, Simon; Yellowlees, Lesley J.; Chemical communications (Cambridge, England)  (2005) 4563–4565; doi:10.1039/b505697g

data_7113348
_publ_section_title
;
 Structural and EPR characterisation of single electron and alkyl transfer
 products from reaction of dimethyl magnesium with bulky alpha-diimine
 ligands.
;
_journal_issue                   36
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4563
_journal_page_last               4565
_journal_paper_doi               10.1039/b505697g
_journal_year                    2005
_chemical_formula_moiety         '[Mg2Me2L2]1.25C6H14'
_chemical_formula_sum            'C81.5 H103.5 Mg2 N4'
_chemical_formula_weight         1187.80
_chemical_name_common
'((Mg((2,6-iPr2Ph)BIAN)(?-Me))2 (2) in paper)'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                93.43(4)
_cell_angle_beta                 106.93(3)
_cell_angle_gamma                100.09(4)
_cell_formula_units_Z            2
_cell_length_a                   14.513(7)
_cell_length_b                   14.781(9)
_cell_length_c                   18.381(9)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     3688(4)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_method       Omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1322
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9159
_diffrn_reflns_theta_full        55.08
_diffrn_reflns_theta_max         55.08
_diffrn_reflns_theta_min         2.53
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.868
_exptl_absorpt_correction_T_min  0.474
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.070
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1289
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.507
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00050(19)
_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   0.962
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     722
_refine_ls_number_reflns         9159
_refine_ls_number_restraints     880
_refine_ls_restrained_S_all      0.928
_refine_ls_R_factor_all          0.1569
_refine_ls_R_factor_gt           0.0970
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2458
_refine_ls_wR_factor_ref         0.2867
_reflns_number_gt                4743
_reflns_number_total             9159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b505697g.txt
_cod_data_source_block           mget99
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1752P)^2^+0.0000P] 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^)+(0.1752P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        3688(3)
_cod_original_sg_symbol_Hall     -P1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C81.50 H103.50 Mg2 N4'
_cod_database_code               7113348