Reversible pressure-induced amorphization of a zeolitic imidazolate framework (ZIF-4)
Thomas Bennett; Petra Simoncic; Stephen Moggach; Fabia Gozzo; Piero Macchi; David Keen; Jin-Chong Tan; Tony Cheetham; Chem.Commun. 47 (2011) 7983–; doi:10.1039/c1cc11985k

data_7106666
_publ_section_title
;
 Reversible pressure-induced amorphization of a zeolitic imidazolate
 framework (ZIF-4)
;
_journal_name_full               Chem.Commun.
_journal_page_first              7983
_journal_paper_doi               10.1039/c1cc11985k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C12 H12 N8 Zn2, C3 H7 N O'
_chemical_formula_sum            'C15 H19 N9 O Zn2'
_chemical_formula_weight         472.14
_chemical_name_common            ZIF-4
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-03-18
_audit_creation_method           CRYSTALS_ver_14.06
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.3486(14)
_cell_length_b                   15.1069(17)
_cell_length_c                   18.3430(19)
_cell_measurement_reflns_used    2065
_cell_measurement_temperature    293
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     4253.2(8)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_diffrn_ambient_pressure         130
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.651
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11913
_diffrn_reflns_theta_full        17.550
_diffrn_reflns_theta_max         23.400
_diffrn_reflns_theta_min         2.916
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.278
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.58
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1920
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.90
_refine_diff_density_min         -0.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.8034
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         1990
_refine_ls_number_restraints     240
_refine_ls_R_factor_all          0.1810
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.0001219
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.34 0.979 -0.133
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2249
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.2249
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              14
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                262
_reflns_number_total             2025
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   5.06
_oxford_diffrn_Wilson_scale      423.22
_oxford_refine_ls_r_factor_ref   0.1810
_oxford_refine_ls_scale          0.036855(14)
_oxford_reflns_number_all        1990
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'tst9008 in Pbca'
_cod_data_source_file            c1cc11985k.txt
_cod_data_source_block           phaseI_13
_cod_original_formula_sum        'C15 H19 N9 O1 Zn2'
_cod_database_code               7106666