Ancillary Ligand Effect on the Properties of "Mg(thd)2" and Crystal Structures of [Mg(thd)2(ethylenediamine)]2, [Mg(thd)2(tmeda)], and [Mg(thd)2(trien)]1
Timo Hatanpää; Jarno Kansikas; Ilpo Mutikainen; Markku Leskelä; Inorganic Chemistry 40 (2001) 788–794; doi:10.1021/ic000310i

data_4319224
_publ_section_title
;
 Ancillary Ligand Effect on the Properties of "Mg(thd)2" and Crystal
 Structures of [Mg(thd)2(ethylenediamine)]2, [Mg(thd)2(tmeda)], and
 [Mg(thd)2(trien)]1
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              788
_journal_page_last               794
_journal_paper_doi               10.1021/ic000310i
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C24 H46 Mg N2 O4'
_chemical_formula_weight         450.94
_chemical_melting_point          425.15
_chemical_name_common
bis(2,2,6,6-tetramethyl-3,5-heptanedione)magnesium(II)(ethylenediamine)
_chemical_name_systematic
; 
 bis(2,2,6,6-tetramethyl-3,5-heptanedione)magnesium(II)(1,2-ethanediamine) 
;
_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                93.08(3)
_cell_angle_beta                 91.45(3)
_cell_angle_gamma                107.44(3)
_cell_formula_units_Z            4
_cell_length_a                   10.372(2)
_cell_length_b                   14.790(3)
_cell_length_c                   19.588(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      5
_cell_volume                     2859.9(11)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection       'MSC/AFC Diffractometer Control Software'
_computing_data_reduction        'TEXSAN (Molecular Structure Corporation)'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.821
_diffrn_measured_fraction_theta_max 0.821
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       \w/2\q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0550
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            7905
_diffrn_reflns_theta_full        24.62
_diffrn_reflns_theta_max         24.62
_diffrn_reflns_theta_min         2.61
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.273
_refine_diff_density_min         -0.310
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0063(12)
_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   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         7905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1039
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.056
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1017P)^2^+0.7482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1698
_refine_ls_wR_factor_ref         0.1900
_reflns_number_gt                5542
_reflns_number_total             7905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000310i_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'None' changed to
'none' 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^)+(0.1017P)^2^+0.7482P] 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^)+(0.1017P)^2^+0.7482P] 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        2859.9(10)
_cod_database_code               4319224