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_4502024
_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_absolute_configuration unk
_chemical_formula_moiety
'C28 H18 Cd1.5 O9 Si, C2 H8 N, 4(C4 H9 N O), 4(H2 O)'
_chemical_formula_sum            'C46 H70 Cd1.5 N5 O17 Si'
_chemical_formula_weight         1161.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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            8
_cell_length_a                   15.62062(10)
_cell_length_b                   27.71138(15)
_cell_length_c                   22.84956(14)
_cell_measurement_reflns_used    27363
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.1838
_cell_measurement_theta_min      1.9319
_cell_volume                     9890.86(10)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0646
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            75521
_diffrn_reflns_theta_full        71.64
_diffrn_reflns_theta_max         71.64
_diffrn_reflns_theta_min         3.19
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) 
(compiled May  8 2007,13:10:02) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4824
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
 SQUEEZE suggests 2007 e/cell.
 Me2NH2 = C2H8N = 27e; dma = C4H9NO = 48e. H2O = 10e.
 Chemist says the missing cation should be Me2NH2.
 Mother liguor was dma:H2O in 1:1 ratio. dma+H2O = 58e.
 Need one Me2NH2 per asu, so 2007-(27x8) = 1791e or 224 e/asu for solvent.
 4dma:H2O = 232e, so this was used.
;
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 4345 Friedel pairs'
_refine_ls_abs_structure_Flack   0.473(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.966
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         9564
_refine_ls_number_restraints     758
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0410P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0776
_reflns_number_gt                7718
_reflns_number_total             9564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1008768_si_001.cif
_cod_data_source_block           IMP-10
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_cell_volume        9890.87(10)
_cod_original_sg_symbol_H-M      C222(1)
_cod_original_formula_sum        'C46 H70 Cd1.50 N5 O17 Si'
_cod_database_code               4502024