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_4502025
_publ_section_title
;
 Structural Diversity in Metal&#x2212;Organic Frameworks Built from Rigid
 Tetrahedral [Si(p-C6H4CO2)4]4&#x2212;Struts
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_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         'C28 H16 O8 Si Zn1.5, C2 H8 N, 3(C3 H7 N O)'
_chemical_formula_sum            'C39 H45 N4 O11 Si Zn1.5'
_chemical_formula_weight         871.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 114.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.205(5)
_cell_length_b                   13.701(4)
_cell_length_c                   25.803(9)
_cell_measurement_reflns_used    51532
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      70.7432
_cell_measurement_theta_min      3.2014
_cell_volume                     8109(4)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'OD Xcalibur PX Ultra'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54248
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0181
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            98398
_diffrn_reflns_theta_full        71.06
_diffrn_reflns_theta_max         71.06
_diffrn_reflns_theta_min         3.76
_exptl_absorpt_coefficient_mu    1.971
_exptl_absorpt_correction_T_max  1.09225
_exptl_absorpt_correction_T_min  0.90802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) 
(compiled May 11 2006,17:41:17) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
 SQUEEZE suggests 1164 e/cell, or 145.5 e/asu.
 Chemist says the missing cation should be Me2NH2 
 The cation Me2NH2 = C2H8N = 27e. The solvent dmf = C3H7NO = 40e.
 145.5 - 27 = 118.5e. 3dmf = 120e, so solvent modelled as 3dmf.
;
_refine_diff_density_max         1.545
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         7815
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1578P)^2^+11.2898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2337
_refine_ls_wR_factor_ref         0.2389
_reflns_number_gt                6232
_reflns_number_total             7815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1008768_si_001.cif
_cod_data_source_block           IMP-11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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      C2/c
_cod_original_formula_sum        'C39 H45 N4 O11 Si Zn1.50'
_cod_database_code               4502025