Synthesis, Structural Characterization, and Transmetalation Reactions of a Tetranuclear Magnesium Silsesquioxane Complex
R. W. J. M. Hanssen; A. Meetsma; R. A. van Santen; H. C. L. Abbenhuis; Inorganic Chemistry 40 (2001) 4049–4052; doi:10.1021/ic0004131

data_4319996
_publ_contact_author_address
;
     Crystal Structure Center,
     Chemical Physics,
     Materials Science Center,
     Groningen University,
     Nijenborgh 4,
     NL-9747 AG Groningen,
     The Netherlands.
;
_publ_contact_author_email       A.Meetsma@fwn.rug.nl
_publ_contact_author_fax         '+31 50 3634441'
_publ_contact_author_name
;
   Drs. A. Meetsma
;
_publ_contact_author_phone       '+31 50 3634368'
_publ_section_title
;
 Synthesis, Structural Characterization, and Transmetalation Reactions of
 a Tetranuclear Magnesium Silsesquioxane Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4049
_journal_page_last               4052
_journal_paper_doi               10.1021/ic0004131
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'by syntheses'
_chemical_formula_moiety         'C78 H142 Cl2 Mg4 O26 Si14, 4(C4 H8 O)'
_chemical_formula_sum            'C102 H190 Cl2 Mg4 O32 Si14'
_chemical_formula_weight         2489.93
_chemical_name_systematic
;
 ?
;
_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_date             1999-02-03
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 113.229(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.744(1)
_cell_length_b                   26.526(2)
_cell_length_c                   16.917(1)
_cell_measurement_temperature    153
_cell_volume                     6492.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
 PLUTO (Meetsma, 1997)
 ORTEP (Burnett et al., 1996)
 PLATON (Spek, 1994, 1996)
;
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      153
_diffrn_measurement_device_type
;
      SMART CCD  area detector diffractometer
;
_diffrn_measurement_method       omega-scans
_diffrn_radiation_detector
;
    CCD area detector
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine focus sealed Siemens Mo tube '
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            31707
_diffrn_reflns_reduction_process
;
 Intensity data were corrected for Lorentz and polarization  effects, scale
 variation and not for absorption and reduced to F~o~^2^
;
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .27
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, 1999'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         .456
_refine_diff_density_min         -.312
_refine_diff_density_rms         .072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11045
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.1194
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0927P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1502
_refine_ls_wR_factor_ref         0.1732
_reflns_number_gt                6327
_reflns_number_total             11045
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0004131.cif
_cod_data_source_block           c47h87cl
_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 'multiscan'
changed to 'multi-scan' 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:

'_exptl_crystal_density_meas' value 'Not Measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0927P)^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^)+(0.0927P)^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 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4319996