Structural Diversity in Metal−Organic Frameworks Built from Rigid Tetrahedral [Si(p-C6H4CO2)4]4−Struts
Davies, Robert P.; Less, Rob; Lickiss, Paul D.; Robertson, Karen; White, Andrew J. P.; Crystal Growth & Design 10 (2010) 4571–; doi:10.1021/cg1008768

data_4502023
_publ_section_title
;
 Structural Diversity in Metal&#x2212;Organic Frameworks Built from Rigid
 Tetrahedral [Si(p-C6H4CO2)4]4&#x2212;Struts
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4571
_journal_paper_doi               10.1021/cg1008768
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety
'C3.5 H2.5 O1.25 Si0.125 Cu0.25, 1.5(C4 H9 N O)'
_chemical_formula_sum            'C9.5 H16 Cu0.25 N1.5 O2.75 Si0.125'
_chemical_formula_weight         214.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           131
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4c 2'
_symmetry_space_group_name_H-M   'P 42/m m c'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   12.3710(12)
_cell_length_b                   12.3710(12)
_cell_length_c                   24.0689(10)
_cell_measurement_reflns_used    2881
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.0575
_cell_measurement_theta_min      1.8307
_cell_volume                     3683.5(5)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1683
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15855
_diffrn_reflns_theta_full        71.50
_diffrn_reflns_theta_max         74.20
_diffrn_reflns_theta_min         3.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.607
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Oxford Diffraction Ltd., 
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) 
(compiled May  6 2009,17:20:42) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
;
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'blocky needles'
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
 SQUEEZE suggests 1128e/cell = 70e/asu
 Solvent = dma = C4H9NO = 48e. 1.5dma = 72e, so this was used as the
 solvent present
;
_refine_diff_density_max         2.507
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.393
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         2036
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.408
_refine_ls_R_factor_all          0.2156
_refine_ls_R_factor_gt           0.1879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4202
_refine_ls_wR_factor_ref         0.4358
_reflns_number_gt                1278
_reflns_number_total             2036
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1008768_si_001.cif
_cod_data_source_block           IMP-9
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P4(2)/mmc
_cod_original_formula_sum        'C9.50 H16 Cu0.25 N1.50 O2.75 Si0.125'
_cod_database_code               4502023