#------------------------------------------------------------------------------
#$Date: 2021-10-01 01:16:56 +0300 (Fri, 01 Oct 2021) $
#$Revision: 269405 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564772.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1564772
loop_
_publ_author_name
'Turner, Gemma F.'
'McKellar, Scott C.'
'Allan, David R.'
'Cheetham, Anthony K.'
'Henke, Sebastian'
'Moggach, Stephen A.'
_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       ω
_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/[σ²(F²) + ( 0.00P)² +23.55P] 
 ,where P=(max(Fo²,0) + 2Fc²)/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>2.0σ(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)
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-y,x,z
y,-x,-z
-x,-y,z
x,y,-z
y,-x,z
-y,x,-z
-x,y,z
x,-y,-z
y,x,z
-y,-x,-z
x,-y,z
-x,y,-z
-y,-x,z
y,x,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Zn1 Zn 0.5000 0.5000 0.3469(2) 0.0247 1.0000 Uani S T . . . .
C1 C 0.2638(10) 0.5000 0.5000 0.0305 1.0000 Uani DS TU . . . .
C2 C 0.1273(10) 0.5000 0.5000 0.0300 1.0000 Uani DS TU . . . .
C3 C 0.0633(4) 0.5000 0.3777(8) 0.0513 1.0000 Uani DS TU . . . .
C4 C 0.4115(6) 0.4115(6) 0.0800(5) 0.0246 0.3750 Uani DS U . . . .
C5 C 0.5000 0.3778(9) 0.0787(5) 0.0244 0.3750 Uani DS U . . . .
N1 N 0.5000 0.5000 0.1350 0.0236 1.0000 Uani D U . . . .
O1 O 0.3177(7) 0.5000 0.3853(6) 0.0383 1.0000 Uani DS TU . . . .
H13 H 0.3304 0.4392 0.1006 0.0468 0.3750 Uiso R . . . . .
H32 H 0.1059 0.5000 0.2926 0.0597 1.0000 Uiso RS . . . . .
H51 H 0.5715 0.3359 0.1104 0.0293 0.3750 Uiso R . . . . .
H52 H 0.4288 0.3359 0.1104 0.0293 0.3750 Uiso R . . . . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Zn 0.2839 1.4301 14.0743 3.2655 7.0318 0.2333 5.1652 10.3163 2.4100 58.7097
1.3041 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Zn1 2_666 Zn1 . O1 3_655 79.44(18) yes
Zn1 2_666 Zn1 . O1 5_665 79.44(18) yes
O1 3_655 Zn1 . O1 5_665 88.07(7) yes
Zn1 2_666 Zn1 . O1 7_565 79.44(18) yes
O1 3_655 Zn1 . O1 7_565 158.9(4) yes
O1 5_665 Zn1 . O1 7_565 88.07(7) yes
Zn1 2_666 Zn1 . O1 . 79.44(18) yes
O1 3_655 Zn1 . O1 . 88.07(7) yes
O1 5_665 Zn1 . O1 . 158.9(4) yes
O1 7_565 Zn1 . O1 . 88.07(7) yes
O1 6_556 C1 . C2 . 118.0(6) yes
O1 6_556 C1 . O1 . 124.1(11) yes
C2 . C1 . O1 . 118.0(6) yes
C1 . C2 . C3 6_556 120.6(5) yes
C1 . C2 . C3 . 120.6(5) yes
C3 6_556 C2 . C3 . 118.8(10) yes
C3 5_565 C3 . C2 . 120.6(5) yes
C3 5_565 C3 . H32 . 119.5 no
C2 . C3 . H32 . 119.9 no
C4 6_555 C4 . H13 11_555 102.0 no
C4 6_555 C4 . H52 11_555 109.1 no
H13 11_555 C4 . H52 11_555 114.7 no
C4 6_555 C4 . H51 7_565 109.1 no
H13 11_555 C4 . H51 7_565 114.5 no
H52 11_555 C4 . H51 7_565 0.2 no
C4 6_555 C4 . H51 9_655 109.1 no
H13 11_555 C4 . H51 9_655 9.3 no
H52 11_555 C4 . H51 9_655 106.1 no
H51 7_565 C4 . H51 9_655 105.9 no
C4 6_555 C4 . N1 . 111.2(2) yes
H13 11_555 C4 . N1 . 109.0 no
H52 11_555 C4 . N1 . 110.5 no
H51 7_565 C4 . N1 . 110.6 no
H51 9_655 C4 . N1 . 110.6 no
C4 6_555 C4 . H13 . 102.0 no
H13 11_555 C4 . H13 . 122.9 no
H52 11_555 C4 . H13 . 9.2 no
H51 7_565 C4 . H13 . 9.3 no
H51 9_655 C4 . H13 . 114.5 no
C4 6_555 C4 . H52 . 109.1 no
H13 11_555 C4 . H52 . 9.2 no
H52 11_555 C4 . H52 . 106.3 no
H51 7_565 C4 . H52 . 106.1 no
H51 9_655 C4 . H52 . 0.2 no
N1 . C4 . H13 . 109.0 no
N1 . C4 . H52 . 110.5 no
H13 . C4 . H52 . 114.7 no
C5 6_555 C5 . H51 9_655 108.7 no
C5 6_555 C5 . H52 9_655 108.8 no
H51 9_655 C5 . H52 9_655 109.5 no
C5 6_555 C5 . N1 . 112.2(2) yes
H51 9_655 C5 . N1 . 108.8 no
H52 9_655 C5 . N1 . 108.8 no
C5 6_555 C5 . H51 . 108.7 no
H51 9_655 C5 . H51 . 109.6 no
H52 9_655 C5 . H51 . 0.1 no
N1 . C5 . H51 . 108.8 no
C5 6_555 C5 . H52 . 108.8 no
H51 9_655 C5 . H52 . 0.1 no
H52 9_655 C5 . H52 . 109.3 no
N1 . C5 . H52 . 108.8 no
H51 . C5 . H52 . 109.5 no
C4 5_665 N1 . C4 7_565 82.45(15) yes
C4 5_665 N1 . C4 3_655 82.45(15) yes
C4 7_565 N1 . C4 3_655 137.5(5) yes
C4 5_665 N1 . C4 . 137.5(5) yes
C4 7_565 N1 . C4 . 82.45(15) yes
C4 3_655 N1 . C4 . 82.45(15) yes
C4 5_665 N1 . C5 11_555 118.2(2) yes
C4 7_565 N1 . C5 11_555 41.66(5) yes
C4 3_655 N1 . C5 11_555 118.2(2) yes
C4 . N1 . C5 11_555 41.66(5) yes
C4 5_665 N1 . C5 . 118.2(2) yes
C4 7_565 N1 . C5 . 118.2(2) yes
C4 3_655 N1 . C5 . 41.66(5) yes
C4 . N1 . C5 . 41.66(5) yes
C5 11_555 N1 . C5 . 81.78(17) yes
C4 5_665 N1 . C5 3_655 41.66(5) yes
C4 7_565 N1 . C5 3_655 118.2(2) yes
C4 3_655 N1 . C5 3_655 41.66(5) yes
C4 . N1 . C5 3_655 118.2(2) yes
C5 11_555 N1 . C5 3_655 135.6(5) yes
C4 5_665 N1 . C5 5_665 41.66(5) yes
C4 7_565 N1 . C5 5_665 41.66(5) yes
C4 3_655 N1 . C5 5_665 118.2(2) yes
C4 . N1 . C5 5_665 118.2(2) yes
C5 11_555 N1 . C5 5_665 81.78(17) yes
C5 . N1 . C5 3_655 81.78(17) yes
C5 . N1 . C5 5_665 135.6(5) yes
C5 3_655 N1 . C5 5_665 81.78(17) yes
Zn1 . O1 . C1 . 128.5(7) yes
C5 . H51 . C4 3_655 67.8 no
C5 . H52 . C4 . 67.9 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 . Zn1 2_666 2.977(4) yes
Zn1 . O1 3_655 2.036(8) yes
Zn1 . O1 5_665 2.036(8) yes
Zn1 . O1 7_565 2.036(8) yes
Zn1 . O1 . 2.036(8) yes
C1 . O1 6_556 1.262(6) yes
C1 . C2 . 1.499(8) yes
C1 . O1 . 1.262(6) yes
C2 . C3 6_556 1.381(7) yes
C2 . C3 . 1.381(7) yes
C3 . C3 5_565 1.390(9) yes
C3 . H32 . 0.950 no
C4 . C4 6_555 1.556(9) yes
C4 . H13 11_555 0.962 no
C4 . H52 11_555 0.901 no
C4 . H51 7_565 0.901 no
C4 . H51 9_655 0.901 no
C4 . N1 . 1.475(9) yes
C4 . H13 . 0.962 no
C4 . H52 . 0.901 no
C5 . C5 6_555 1.529(9) yes
C5 . H51 9_655 0.961 no
C5 . H52 9_655 0.959 no
C5 . N1 . 1.449(9) yes
C5 . H51 . 0.961 no
C5 . H52 . 0.959 no
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.002 -0.002 -0.020 719 202 '7.8 (C2 O H6)'
loop_
_oxford_refln_omitted_index_h
_oxford_refln_omitted_index_k
_oxford_refln_omitted_index_l
_oxford_refln_omitted_flag
_oxford_refln_omitted_details
0 4 0 x .
3 11 5 x .
4 7 9 x .
4 6 5 x .
0 3 2 x .
0 4 11 x .
0 0 2 x .
