Polynuclear Magnesium and Magnesium-Titanium Species. Syntheses and Crystal Structures of [Mg4(μ3,η2-ddbfo)2(μ,η2-ddbfo)2(μ,η1-ddbfo)2(η1-ddbfo)2], [Mg4(μ3-OMe)2(μ,η2-ddbfo)2(μ,η1-ddbfo)2(η1-ddbfo)2(CH3OH)5], and [Mg4(μ3,η2-thffo)2(μ,η2-thffo)2(μ,η1-thffo)2{μ-OTi(DIPP)3}2] Aggregates
Piotr Sobota; Józef Utko; Katarzyna Sztajnowska; Jolanta Ejfler; Lucjan B. Jerzykiewicz; Inorganic Chemistry 39 (2000) 235–239; doi:10.1021/ic990542l

data_4300038
_publ_section_title
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Polynuclear Magnesium and Magnesium-Titanium Species. Syntheses and
Crystal Structures of
[Mg4(\m3,\h2-ddbfo)2(\m,\h2-ddbfo)2(\m,\h1-ddbfo)2(\h1-ddbfo)2],
[Mg4(\m3-OMe)2(\m,\h2-ddbfo)2(\m,\h1-ddbfo)2(\h1-ddbfo)2(CH3OH)5], and
[Mg4(\m3,\h2-thffo)2(\m,\h2-thffo)2(\m,\h1-thffo)2{\m-OTi(DIPP)3}2]
Aggregates
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              235
_journal_page_last               239
_journal_paper_doi               10.1021/ic990542l
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C72 H104 Mg4 O21'
_chemical_formula_weight         1402.79
_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                 104.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.323(3)
_cell_length_b                   20.768(4)
_cell_length_c                   27.584(6)
_cell_measurement_reflns_used    3570
_cell_measurement_temperature    100.0(4)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     7397(3)
_computing_cell_refinement       'Kuma KM4 CCD, 1998'
_computing_data_collection       'Kuma KM4 CCD, 1998'
_computing_data_reduction        'Kuma KM4 CCD, 1998'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(4)
_diffrn_measured_fraction_theta_full 0.702
_diffrn_measured_fraction_theta_max 0.702
_diffrn_measurement_device_type  'Kuma KM4 CDD diffractometer'
_diffrn_measurement_method       'Area-detector \w-scan'
_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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            27208
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       0.0004(2)
_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   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     919
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.102
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+12.3176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                9419
_reflns_number_total             9424
_reflns_threshold_expression     >2sigma(I)
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0770P)^2^+12.3176P] 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^)+(0.0770P)^2^+12.3176P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4300038