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_4319226
_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            'C28 H56 Mg N4 O4'
_chemical_formula_weight         537.08
_chemical_melting_point          348.15
_chemical_name_common
;
 bis(2,2,6,6-tetramethyl-3,5-heptanedionate)magnesium(II)
 (triethylenetetramine)
;
_chemical_name_systematic
; 
 bis(2,2,6,6-tetramethyl-3,5-heptanedionate)magnesium(II)
 (triethylenetetramine) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.246(3)
_cell_length_b                   10.850(2)
_cell_length_c                   20.882(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      3
_cell_volume                     3335.6(12)
_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 0.713
_diffrn_measured_fraction_theta_max 0.713
_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    0.0841
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            3983
_diffrn_reflns_theta_full        24.04
_diffrn_reflns_theta_max         24.04
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        0.6
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.004(3)
_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   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         3983
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1712
_refine_ls_R_factor_gt           0.1110
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2896P)^2^+0.8467P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3076
_refine_ls_wR_factor_ref         0.3638
_reflns_number_gt                2304
_reflns_number_total             3983
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000310i_3.cif
_cod_data_source_block           7
_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.

'_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^)+(0.2896P)^2^+0.8467P] 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^)+(0.2896P)^2^+0.8467P] 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        3335.6(11)
_cod_database_code               4319226