Pressure-Induced Cooperative Bond Rearrangement in a Zinc Imidazolate Framework: A High-Pressure Single-Crystal X-Ray Diffraction Study
Elinor C. Spencer; Ross J. Angel; Nancy L. Ross; Brian E. Hanson; Judith A. K. Howard; Journal of the American Chemical Society 131 (2009) 4022–4026; doi:10.1021/ja808531m

data_4104053
_publ_section_title
;
 Pressure-Induced Cooperative Bond Rearrangement in a Zinc Imidazolate
 Framework: A High-Pressure Single-Crystal X-Ray Diffraction Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4022
_journal_page_last               4026
_journal_paper_doi               10.1021/ja808531m
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C12 H12 N8 Zn2'
_chemical_formula_sum            'C12 H12 N8 Zn2'
_chemical_formula_weight         399.04
_chemical_name_common
;
Zinc imidazolate 3D framework
;
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           80
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_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            16
_cell_length_a                   22.7482(3)
_cell_length_b                   22.7482(3)
_cell_length_c                   13.0168(3)
_cell_measurement_pressure       Ambient
_cell_measurement_reflns_used    9176
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      3.101
_cell_volume                     6735.9(2)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction)'
_computing_data_collection       'CrysAlis (Oxford Diffraction)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction)'
_computing_molecular_graphics    'crystal Maker'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXs-97 (Sheldrick, 1997)'
_diffrn_ambient_pressure         Ambient
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 16.0355
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device
;
\k-geometry diffractometer, Gemini, Oxford Diffraction Ltd., 
;
_diffrn_measurement_device_type  'Oxford Diffraction Atlas CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26566
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.11
_diffrn_source_current           40
_diffrn_source_voltage           50
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.856
_exptl_absorpt_correction_T_max  0.797
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.20 (release 21-03-2008 CrysAlis171 .NET)
(compiled Mar 21 2008,15:12:32)
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    1.574
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.1848
_exptl_crystal_size_mid          0.1337
_exptl_crystal_size_min          0.1062
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.255
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5974
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0382
_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^)+(0.0217P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0540
_reflns_number_gt                4816
_reflns_number_total             5974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja808531m_si_002_6.cif
_cod_data_source_block           PostDAC_ZnIm
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4104053