Guest-mediated phase transitions in a flexible pillared-layered metal‒organic framework under high-pressure
Turner, Gemma F.; McKellar, Scott C.; Allan, David R.; Cheetham, Anthony K.; Henke, Sebastian; Moggach, Stephen A.; Chemical Science  (2021) –; doi:10.1039/D1SC03108B

data_1564779
_publ_section_title
;
 Guest-mediated phase transitions in a flexible pillared-layered
 metal--organic framework under high-pressure
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC03108B
_journal_year                    2021
_chemical_formula_moiety         '(C22 H20 N2 O8 Zn2)n. 4(C3H7NO)'
_chemical_formula_sum            'C34 H48 N6 O12 Zn2'
_chemical_formula_weight         863.55
_space_group_IT_number           140
_space_group_name_Hall           '-I 4 2c'
_space_group_name_H-M_alt        'I 4/m c m'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4 2c'
_symmetry_space_group_name_H-M   'I 4/m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2021-05-26
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_audit_update_record
;
2021-06-03 deposited with the CCDC.	2021-09-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1100(10)
_cell_length_b                   15.1100(10)
_cell_length_c                   19.2672(12)
_cell_measurement_reflns_used    4952
_cell_measurement_temperature    298
_cell_measurement_theta_max      18
_cell_measurement_theta_min      3
_cell_volume                     4398.9(5)
_computing_cell_refinement       'USER DEFINED CELL REFINEMENT'
_computing_data_collection       'USER DEFINED DATA COLLECTION'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_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    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_pressure         100000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.759
_diffrn_measured_fraction_theta_max 0.759
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  Synchrotron
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.48590
_diffrn_reflns_av_R_equivalents  0.112
_diffrn_reflns_av_unetI/netI     0.145
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            10160
_diffrn_reflns_theta_full        17.667
_diffrn_reflns_theta_max         17.667
_diffrn_reflns_theta_min         2.184
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.150
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.79
_refine_diff_density_min         -1.28
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9768
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         904
_refine_ls_number_restraints     165
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.1009
_refine_ls_shift/su_max          0.0015416
_refine_ls_shift/su_mean         0.0000748
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.09P)^2^ +59.13P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.3887
_refine_ls_wR_factor_gt          0.3645
_refine_ls_wR_factor_ref         0.1969
_reflns_limit_h_max              13
_reflns_limit_h_min              0
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                575
_reflns_number_total             935
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.77
_oxford_diffrn_Wilson_scale      855.88
_oxford_refine_ls_r_factor_ref   0.1087
_oxford_refine_ls_scale          0.424(2)
_oxford_reflns_number_all        935
_cod_data_source_file            d1sc03108b2.cif
_cod_data_source_block           2_DMF_010GPa
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4398.9(6)
_cod_original_sg_symbol_Hall     '-I 4 2c '
_cod_original_sg_symbol_H-M      'I 4/m c m '
_cod_database_code               1564779
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)