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_4104051
_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'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c 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            16
_cell_length_a                   23.2297(4)
_cell_length_b                   23.2297(4)
_cell_length_c                   12.4296(5)
_cell_measurement_pressure       295000(6000)
_cell_measurement_reflns_used    558
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.59
_cell_measurement_theta_min      2.43
_cell_volume                     6707.2(3)
_computing_cell_refinement       'RED v171.32 (Oxford Diffraction)'
_computing_data_collection       'CCD v171.32 (Oxford Diffraction)'
_computing_data_reduction
;
RED v171.32 (Oxford Diffraction)
Absorb61, Angel (2004) J. Appl. Cryst. 37:486-492
Average v.2.21, Angel (2005)                 
;
_computing_molecular_graphics
;
CrystalMaker V.2.0.6, CrystalMaker Software Ltd.'
;
_computing_structure_refinement
;
shelxl-97 (G.M.Sheldrick, 2008, Acta Cryst., A64,112)
WinGX (L.J Farrugia, 1999, J. Appl. Cryst., 32, 837)
;
_computing_structure_solution
;
shelxs-86 (G.M.Sheldrick, 2008, Acta Cryst., A64,112)
WinGX (L.J Farrugia, 1999, J. Appl. Cryst., 32, 837)
;
_diffrn_ambient_pressure         295000(6000)
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Oxford Diffraction, Xcalibur1 CCD'
_diffrn_measured_fraction_theta_full 0.541
_diffrn_measured_fraction_theta_max 0.539
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur1'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  1.015
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            51091
_diffrn_reflns_reduction_process
; 
Data averaged using Blessing (1987) criteria 
;
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    2.848
_exptl_absorpt_correction_T_max  0.302
_exptl_absorpt_correction_T_min  0.217
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
Gaussian integration over a grid
of 16 x  8 x 16 points =  2048 total grid points
  Based upon method of Burnham (1966)

 Data corrected for diamond-anvil cell absorption
 Note that exptl_absorpt_correction_tmin and _tmax
 the total correction factors applied to the intensities
 The individual factors are: 
         range of dac transmission factors (min-max)      0.307     0.394
         range of gasket transmission (min-max)           0.937     1.000
         range of P media transmission (min-max)          1.000     1.000

 thickness of diamond anvil 1:  1.500 mm, mu =  0.2000 mm-1
       thickness of platten 1:  3.300 mm, mu =  0.0500 mm-1

 thickness of diamond anvil 2:  1.500 mm, mu =  0.2000 mm-1
       thickness of platten 2:  3.300 mm, mu =  0.0500 mm-1

    Gasket shadowing corrections were made based upon
    Gasket thickness = 145.0 microns, radius = 250.0 microns
    Gasket absorption coeff =        30.00 mm-1
    REFLECTION WAS CONSIDERED TOTALLY OBSCURED IF 
 FRACTION CRYSTAL ILLUMINATED WAS LESS THAN 0.20

    Non-absorbing pressure medium
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3200
_exptl_crystal_preparation
;
crystal mounted in a diamond-anvil cell
;
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.096
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(9)
_refine_ls_extinction_coef       'not refined'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     77
_refine_ls_number_reflns         584
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      0.841
_refine_ls_R_factor_all          0.2073
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0447
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                306
_reflns_number_total             3018
_reflns_threshold_expression     'Fsqd > 2.0u(Fsqd)'
_cod_data_source_file            ja808531m_si_002_4.cif
_cod_data_source_block           DAC_P2
_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               4104051
_diffrn_reflns_uneti/neti        0.012