#------------------------------------------------------------------------------
#$Date: 2021-10-01 01:16:56 +0300 (Fri, 01 Oct 2021) $
#$Revision: 269405 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/47/1564781.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_1564781
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 3.9 (C2 O H6)'
_chemical_formula_sum            'C29.8 H49.4 N2 O11.9 Zn2'
_chemical_formula_weight         756.9
_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                   10.91350(4)
_cell_length_b                   10.91350(4)
_cell_length_c                   9.62600(4)
_cell_measurement_reflns_used    24471
_cell_measurement_temperature    298
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     1146.500(8)
_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         101
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.043
_diffrn_reflns_av_unetI/netI     0.055
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24471
_diffrn_reflns_theta_full        26.406
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         2.116
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.09
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             397.4
_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         0.36
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0364
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     31
_refine_ls_number_reflns         745
_refine_ls_number_restraints     73
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.0087092
_refine_ls_shift/su_mean         0.0003984
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² + 0.47P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0668
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0668
_reflns_limit_h_max              9
_reflns_limit_h_min              0
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                718
_reflns_number_total             745
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.53
_oxford_diffrn_Wilson_scale      29.42
_oxford_refine_ls_r_factor_ref   0.0246
_oxford_refine_ls_scale          0.744(3)
_oxford_reflns_number_all        745
_cod_data_source_file            d1sc03108b2.cif
_cod_data_source_block           1_EtOH_0GPa
_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        1146.500(10)
_cod_original_sg_symbol_H-M      'P 4/m m m '
_cod_original_formula_sum        'C29.8 H49.4 O11.9 N2 Zn2'
_cod_database_code               1564781
_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
y,x,-z
-y,-x,z
-x,-y,z
x,y,-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 0.34860(4) 0.0256 1.0000 Uani S T . . . .
C1 C 0.2651(2) 0.5000 0.5000 0.0432 1.0000 Uani S TU . . . .
C2 C 0.1276(3) 0.5000 0.5000 0.0495 1.0000 Uani S TU . . . .
C3 C 0.0635(2) 0.5000 0.3779(2) 0.0858 1.0000 Uani S TU . . . .
C4 C 0.4116(3) 0.4116(3) 0.0802(5) 0.0615 0.3750 Uani S U . . . .
C5 C 0.5000 0.3773(5) 0.0791(5) 0.0605 0.3750 Uani S U . . . .
N1 N 0.5000 0.5000 0.1343 0.0301 1.0000 Uani . U . . . .
O1 O 0.31747(14) 0.5000 0.38492(16) 0.0607 1.0000 Uani S TU . . . .
H13 H 0.3305 0.4393 0.1007 0.0468 0.3750 Uiso R . . . . .
H51 H 0.4292 0.3360 0.1113 0.0743 0.3750 Uiso R . . . . .
H53 H 0.5728 0.3360 0.1113 0.0743 0.3750 Uiso R . . . . .
H32 H 0.1060 0.5000 0.2918 0.1028 1.0000 Uiso RS . . . . .
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_555 80.04(4) yes
Zn1 2_666 Zn1 . O1 8_565 80.04(4) yes
O1 3_555 Zn1 . O1 8_565 160.09(9) yes
Zn1 2_666 Zn1 . O1 10_655 80.04(4) yes
O1 3_555 Zn1 . O1 10_655 88.287(15) yes
O1 8_565 Zn1 . O1 10_655 88.287(15) yes
Zn1 2_666 Zn1 . O1 . 80.04(4) yes
O1 3_555 Zn1 . O1 . 88.287(15) yes
O1 8_565 Zn1 . O1 . 88.287(15) yes
O1 10_655 Zn1 . O1 . 160.09(9) yes
Zn1 2_666 Zn1 . N1 . 179.99 yes
O1 3_555 Zn1 . N1 . 99.96(4) yes
O1 8_565 Zn1 . N1 . 99.95(4) yes
O1 10_655 Zn1 . N1 . 99.95(4) yes
O1 . Zn1 . N1 . 99.96(4) yes
O1 9_566 C1 . C2 . 117.27(13) yes
O1 9_566 C1 . O1 . 125.5(3) yes
C2 . C1 . O1 . 117.27(13) yes
C1 . C2 . C3 9_566 120.79(14) yes
C1 . C2 . C3 . 120.79(14) yes
C3 9_566 C2 . C3 . 118.4(3) yes
C3 10_555 C3 . C2 . 120.79(14) yes
C3 10_555 C3 . H32 . 119.2 no
C2 . C3 . H32 . 120.0 no
C4 13_555 C4 . H13 3_555 101.9 no
C4 13_555 C4 . H51 3_555 109.5 no
H13 3_555 C4 . H51 3_555 114.8 no
C4 13_555 C4 . H53 8_565 109.6 no
H13 3_555 C4 . H53 8_565 113.5 no
H51 3_555 C4 . H53 8_565 1.4 no
C4 13_555 C4 . H53 10_655 109.6 no
H13 3_555 C4 . H53 10_655 10.3 no
H51 3_555 C4 . H53 10_655 105.1 no
H53 8_565 C4 . H53 10_655 103.8 no
C4 13_555 C4 . N1 . 110.89(19) yes
H13 3_555 C4 . N1 . 109.2 no
H51 3_555 C4 . N1 . 110.3 no
H53 8_565 C4 . N1 . 111.3 no
H53 10_655 C4 . N1 . 111.3 no
C4 13_555 C4 . H13 . 101.9 no
H13 3_555 C4 . H13 . 122.9 no
H51 3_555 C4 . H13 . 9.4 no
H53 8_565 C4 . H13 . 10.3 no
H53 10_655 C4 . H13 . 113.5 no
C4 13_555 C4 . H51 . 109.5 no
H13 3_555 C4 . H51 . 9.4 no
H51 3_555 C4 . H51 . 106.3 no
H53 8_565 C4 . H51 . 105.1 no
H53 10_655 C4 . H51 . 1.4 no
N1 . C4 . H13 . 109.2 no
N1 . C4 . H51 . 110.3 no
H13 . C4 . H51 . 114.8 no
C5 5_655 C5 . H53 10_655 108.7 no
C5 5_655 C5 . H51 10_655 109.1 no
H53 10_655 C5 . H51 10_655 110.2 no
C5 5_655 C5 . H51 . 109.1 no
H53 10_655 C5 . H51 . 0.7 no
H51 10_655 C5 . H51 . 109.5 no
C5 5_655 C5 . H53 . 108.7 no
H53 10_655 C5 . H53 . 110.9 no
H51 10_655 C5 . H53 . 0.7 no
H51 . C5 . H53 . 110.2 no
C5 5_655 C5 . N1 . 111.6(2) yes
H53 10_655 C5 . N1 . 108.4 no
H51 10_655 C5 . N1 . 108.8 no
H51 . C5 . N1 . 108.8 no
H53 . C5 . N1 . 108.4 no
C4 8_565 N1 . C4 . 82.70(13) yes
C4 8_565 N1 . C4 14_665 82.70(13) yes
C4 . N1 . C4 14_665 138.2(4) yes
C4 8_565 N1 . C4 10_655 138.2(4) yes
C4 . N1 . C4 10_655 82.70(13) yes
C4 14_665 N1 . C4 10_655 82.70(13) yes
C4 8_565 N1 . C5 11_655 118.88(15) yes
C4 . N1 . C5 11_655 118.88(15) yes
C4 14_665 N1 . C5 11_655 41.80(3) yes
C4 10_655 N1 . C5 11_655 41.80(3) yes
C4 8_565 N1 . C5 15_665 41.80(3) yes
C4 . N1 . C5 15_665 118.88(15) yes
C4 14_665 N1 . C5 15_665 41.80(3) yes
C4 10_655 N1 . C5 15_665 118.88(15) yes
C5 11_655 N1 . C5 15_665 82.20(14) yes
C4 8_565 N1 . C5 3_555 41.80(3) yes
C4 . N1 . C5 3_555 41.80(3) yes
C4 14_665 N1 . C5 3_555 118.88(15) yes
C4 10_655 N1 . C5 3_555 118.88(15) yes
C5 11_655 N1 . C5 3_555 136.8(4) yes
C4 8_565 N1 . Zn1 . 110.89(19) yes
C4 . N1 . Zn1 . 110.89(19) yes
C4 14_665 N1 . Zn1 . 110.89(19) yes
C4 10_655 N1 . Zn1 . 110.89(19) yes
C5 11_655 N1 . Zn1 . 111.6(2) yes
C4 8_565 N1 . C5 . 118.88(15) yes
C4 . N1 . C5 . 41.80(3) yes
C4 14_665 N1 . C5 . 118.88(15) yes
C4 10_655 N1 . C5 . 41.80(3) yes
C5 11_655 N1 . C5 . 82.20(14) yes
C5 15_665 N1 . C5 3_555 82.20(14) yes
C5 15_665 N1 . Zn1 . 111.6(2) yes
C5 3_555 N1 . Zn1 . 111.6(2) yes
C5 15_665 N1 . C5 . 136.8(4) yes
C5 3_555 N1 . C5 . 82.20(14) yes
Zn1 . N1 . C5 . 111.6(2) yes
Zn1 . O1 . C1 . 127.23(15) yes
C5 . H51 . C4 . 68.2 no
C5 . H53 . C4 11_655 67.6 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 2.9147(7) yes
Zn1 . O1 3_555 2.0225(15) yes
Zn1 . O1 8_565 2.0225(15) yes
Zn1 . O1 10_655 2.0225(15) yes
Zn1 . O1 . 2.0225(15) yes
Zn1 . N1 . 2.0633(3) yes
C1 . O1 9_566 1.2463(19) yes
C1 . C2 . 1.500(4) yes
C1 . O1 . 1.2463(19) yes
C2 . C3 9_566 1.368(3) yes
C2 . C3 . 1.368(3) yes
C3 . C3 10_555 1.385(5) yes
C3 . H32 . 0.950 no
C4 . C4 13_555 1.543(9) yes
C4 . H13 3_555 0.956 no
C4 . H51 3_555 0.898 no
C4 . H53 8_565 0.894 no
C4 . H53 10_655 0.894 no
C4 . N1 . 1.461(5) yes
C4 . H13 . 0.956 no
C4 . H51 . 0.898 no
C5 . C5 5_655 1.524(10) yes
C5 . H53 10_655 0.965 no
C5 . H51 10_655 0.947 no
C5 . H51 . 0.947 no
C5 . H53 . 0.965 no
C5 . N1 . 1.440(5) yes
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 -0.021 695 102 '3.9 (C2 O H6) '
