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_1564772
_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 H26 N2 O8 Zn2)n 7.8 (C2 O H6)'
_chemical_formula_sum            'C37.6 H72.8 N2 O15.8 Zn2'
_chemical_formula_weight         936.56
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m 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            1
_cell_length_a                   10.9805(16)
_cell_length_b                   10.9805(16)
_cell_length_c                   9.7220(19)
_cell_measurement_reflns_used    3660
_cell_measurement_temperature    298
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1172.2(3)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_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         310000
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.581
_diffrn_measured_fraction_theta_max 0.581
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_av_unetI/netI     0.064
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4042
_diffrn_reflns_theta_full        25.031
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         2.798
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.09
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             498.8
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
see text for details
;
_refine_diff_density_max         1.89
_refine_diff_density_min         -1.17
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         379
_refine_ls_number_restraints     78
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0762
_refine_ls_shift/su_max          0.0091720
_refine_ls_shift/su_mean         0.0003097
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.00P)^2^ +23.55P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2024
_refine_ls_wR_factor_gt          0.1709
_refine_ls_wR_factor_ref         0.1895
_reflns_limit_h_max              5
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                333
_reflns_number_total             386
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.24
_oxford_diffrn_Wilson_scale      37.55
_oxford_refine_ls_r_factor_ref   0.0938
_oxford_refine_ls_scale          0.2422(9)
_oxford_reflns_number_all        386
_cod_data_source_file            d1sc03108b2.cif
_cod_data_source_block           1_EtOH_031GPa
_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        1172.2(4)
_cod_original_sg_symbol_H-M      'P 4/m m m '
_cod_original_formula_sum        'C37.6 H72.8 O15.8 N2 Zn2'
_cod_database_code               1564772
_platon_squeeze_void_probe_radius 1.20
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)