Microporous metal‒organic frameworks built from rigid tetrahedral tetrakis(4-tetrazolylphenyl)silane connectors
Timokhin, I.; White, A. J. P.; Lickiss, P. D.; Pettinari, C.; Davies, R. P.; CrystEngComm  (2014) –; doi:10.1039/c4ce00486h

data_7215227
_publ_section_title
;
 Microporous metal--organic frameworks built from rigid tetrahedral
 tetrakis(4-tetrazolylphenyl)silane connectors
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/c4ce00486h
_journal_year                    2014
_chemical_formula_moiety         'C40 H44 Cd2 N20 O4 Si, 16(C3 H7 N O)'
_chemical_formula_sum            'C88 H156 Cd2 N36 O20 Si'
_chemical_formula_weight         2291.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           230
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-I 4bd 2c 3'
_symmetry_space_group_name_H-M   'I a -3 d'
_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            24
_cell_length_a                   36.97447(15)
_cell_length_b                   36.97447(15)
_cell_length_c                   36.97447(15)
_cell_measurement_reflns_used    51071
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.2512
_cell_measurement_theta_min      1.6883
_cell_volume                     50548.2(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
_diffrn_detector_area_resol_mean 8.2556
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0793
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            161857
_diffrn_reflns_theta_full        72.40
_diffrn_reflns_theta_max         72.40
_diffrn_reflns_theta_min         2.93
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.047
_exptl_absorpt_correction_T_max  0.588
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) 
(compiled Aug  3 2011,13:03:54) 
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            Colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             28944
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_platon_squeeze_details
;
 SQUEEZE suggested 15066 e/cell = 156.9 e/asu.
 Before SQUEEZE, the solvent looked like dmf (C3H7NO) = 40e.
 4dmf = 160e so this was used as the solvent present.
 4dmf per asu = 16dmf per LCd2 moiety
 
 So, atom list low by 4(C3H7NO) = C12 H28 N4 O4,
 and UNIT low by C1152 H2688 N384 O384,
 i.e. C960 H1056 N480 O96 Si24 Cd48
;
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.599
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         4182
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0523P)^2^+127.0912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1348
_reflns_number_gt                3535
_reflns_number_total             4182
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00486h2.cif
_cod_data_source_block           IMP-17Cd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      Ia-3d
_cod_database_code               7215227