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_7215225
_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         'C68 H61 Cl Mn4 N36 O4 Si2, 20(C3 H7 N O)'
_chemical_formula_sum            'C128 H201 Cl Mn4 N56 O24 Si2'
_chemical_formula_weight         3219.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           136
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4n 2n'
_symmetry_space_group_name_H-M   'P 42/m n m'
_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            2
_cell_length_a                   18.8266(5)
_cell_length_b                   18.8266(5)
_cell_length_c                   25.4638(17)
_cell_measurement_reflns_used    3726
_cell_measurement_temperature    173
_cell_measurement_theta_max      72.2041
_cell_measurement_theta_min      2.3449
_cell_volume                     9025.4(7)
_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 0.981
_diffrn_measured_fraction_theta_max 0.977
_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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16838
_diffrn_reflns_theta_full        72.00
_diffrn_reflns_theta_max         72.35
_diffrn_reflns_theta_min         2.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.085
_exptl_absorpt_correction_T_max  0.742
_exptl_absorpt_correction_T_min  0.584
_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            'Pale yellow'
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubes
_exptl_crystal_F_000             3396
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
 Due to the severe disorder across symmetry, only the oxygen atoms of the
 coordinated solvent molecules could be reliably located. From the looks
 of the electron density maps, combined with the solvent list given by the
 chemist, the most likely solvent is dmf (C3H7NO).
 So, at the time of running SQUEEZE, the asu contents were low by
 0.5(C3H7N). However, SQUEEZE does not remove electron denisty that is
 within bonding distance of defined atoms, so the contribution of the
 carbonyl carbon would not be removed, meaning that 0.5(C2H7N) = 13 e/asu
 of that removed by SQUEEZE would be due to the coordinated solvent.
 
 SQUEEZE suggested 1830 e/cell = 114.4 e/asu.
 As detailed above, the disorder of the coordinated solvent accounts for
 13 e/asu of this, leaving 101.4 e/asu for the included solvent.
 The included solvent is presumed to be dmf (C3H7NO) = 40e.
 2.5dmf = 100e so this was used as the solvent present.
 2.5dmf per asu = 20dmf per Mn4 unit.
 
 So, atom list low by 0.125(H) + 0.5(C3H7N) 2.5(C3H7NO)
 = H0.125+(C1.5 H3.5 N0.5)+(C7.5 H17.5 N2.5 O2.5)
 = C9 H21.125 N3 O2.5, and UNIT low by C144 H338 N48 O40,
 i.e. C112 H64 N64 O8 Cl2 Mn8 Si4
;
_refine_diff_density_max         0.625
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         4666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0841
_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^)+(0.1563P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2599
_refine_ls_wR_factor_ref         0.2943
_reflns_number_gt                2075
_reflns_number_total             4666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce00486h2.cif
_cod_data_source_block           IMP-16Mn
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_cell_volume        9025.4(8)
_cod_original_sg_symbol_H-M      P4(2)/mnm
_cod_database_code               7215225