Templated synthesis of zirconium(IV)-based metal-organic layers (MOLs) with accessible chelating sites
Gimeno-Fonquernie, Pol; Liang, W.; Albalad, Jorge; Kuznicki, Andrew; Price, Jason; Bloch, Eric D.; Doonan, Christian J.; Sumby, Christopher J.; Chemical Communications  (2022) –; doi:10.1039/D1CC06443F

data_7129420
_publ_section_title
;
 Templated synthesis of zirconium(IV)-based metal-organic layers (MOLs)
 with accessible chelating sites
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06443F
_journal_year                    2022
_chemical_formula_moiety
'C10 H6 N4 O9 Zr1.5, C7.25 H4.5 N3 O7 Zr1.5, 0.5(C3 H7 N O), C1.75 H1.5 N'
_chemical_formula_sum            'C21.5 H16.5 N8.5 O22.5 Zr3'
_chemical_formula_weight         1027.59
_chemical_name_common            UAM-1
_space_group_crystal_system      orthorhombic
_space_group_IT_number           38
_space_group_name_Hall           'A 2 -2'
_space_group_name_H-M_alt        'A m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2021-11-01 deposited with the CCDC.	2021-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.017(4)
_cell_length_b                   23.361(5)
_cell_length_c                   21.208(4)
_cell_measurement_reflns_used    106441
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.173
_cell_measurement_theta_min      1.038
_cell_volume                     9422(3)
_computing_cell_refinement       'AS QEGUI'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean '13.3 (Dectris Eiger detectors)'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type
;
N. P. Cowieson, D. Aragao, M. Clift, D. J. Ericsson, C. Gee, 
S. J. Harrop, N. Mudie, S. Panjikar, J. R. Price, A. Riboldi-
Tunnicliffe, R. Williamson and T. Caradoc-Davies, MX1: a 
bending-magnet crystallography beamline serving both chemical 
and macromolecular crystallography communities at the 
Australian Synchrotron, J. Synchrotron Rad. (2015). 22, 187-190.
;
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            106441
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.868
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         29.173
_diffrn_reflns_theta_min         1.038
_exptl_absorpt_coefficient_mu    3.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             4040
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.338
_refine_diff_density_min         -1.304
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.508(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         12746
_refine_ls_number_restraints     442
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2614
_refine_ls_wR_factor_ref         0.2837
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.841
_reflns_number_gt                10168
_reflns_number_total             12746
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06443f2.cif
_cod_data_source_block           test
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C21.50 H16.50 N8.50 O22.50 Zr3'
_cod_database_code               7129420
_shelx_shelxl_version_number     2018/3
_diffrn_measurement_detector_type 'Dectris Eiger2 9M'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.492
 0.508
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Shared sites
{C74A, C74B}
{C50, C50A}
4. Restrained distances
 C44-C46
 1.42 with sigma of 0.02
 C54-C56
 1.42 with sigma of 0.02
 C44A-C46A_$1
 1.5 with sigma of 0.02
 C56A-O57A
 1.3 with sigma of 0.02
 C56A-O58A
 1.3 with sigma of 0.02
 O57-C56
 1.28 with sigma of 0.02
 O58-C56
 1.28 with sigma of 0.02
 O47-C46
 1.28 with sigma of 0.02
 O48-C46
 1.28 with sigma of 0.02
5. Uiso/Uaniso restraints and constraints
C31 \\sim N41 \\sim N42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim O47 \\sim
O48: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C31A \\sim N41A \\sim N42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim
O47A \\sim O48A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
N51A \\sim N52A \\sim C53A \\sim C54A \\sim C55A \\sim C56A \\sim O57A \\sim
O58A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within
2A
N51 \\sim N52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim O57 \\sim O58:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Zr4 \\sim Zr5 \\sim Zr6 \\sim O14: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uanis(C50) = Uanis(C50A)
Uanis(C56A) = Uanis(O57A) = Uanis(O58A)
Uanis(C31) = Uanis(C31A)
Uanis(C74A) = Uanis(C74B)
6. Rigid body (RIGU) restrains
 C31, N41, N42, C43, C44, C45, C46, O47, O48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31A, N41A, N42A, C43A, C44A, C45A, C46A, O47A, O48A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N51A, N52A, C53A, C54A, C55A, C56A, O57A, O58A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N51, N52, C53, C54, C55, C56, O57, O58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Zr4, Zr5, Zr6, O14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(C74B)=Sof(O75B)=1-FVAR(1)
 Sof(C74A)=Sof(O75A)=FVAR(1)
 Fixed Sof: N51(0.5) N52(0.5) C53(0.5) H53(0.5) C54(0.5) C55(0.5) H55(0.5)
 Zr4(0.5) Zr5(0.25) Zr6(0.25) Zr7(0.5) O9(0.5) O10(0.25) O11(0.25) O12(0.25)
 O13(0.25) O14(0.5) O57A(0.5) O47A(0.5) O58A(0.5) O48A(0.5) C31(0.25)
 H31A(0.25) H31B(0.25) N42(0.5) N41(0.5) C45(0.5) H45(0.5) C44(0.5) C43(0.5)
 H43(0.5) C46(0.5) O47(0.5) O48(0.5) C50(0.25) H50A(0.25) H50B(0.25) C56(0.5)
 O57(0.5) O58(0.5) H65B(0.5) H65C(0.5) O77(0.5) O81(0.5) C56A(0.5) N51A(0.5)
 C55A(0.5) H55A(0.5) C54A(0.5) C53A(0.5) H53A(0.5) N52A(0.5) C50A(0.25)
 H50C(0.25) H50D(0.25) N41A(0.5) N42A(0.5) C43A(0.5) H43A(0.5) C44A(0.5)
 C45A(0.5) H45A(0.5) C46A(0.5) C31A(0.25) H31C(0.25) H31D(0.25) H64B(0.5)
 H64C(0.5)
8.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C31(H31A,H31B), C50(H50A,H50B), C50A(H50C,H50D), C31A(H31C,H31D)
8.b Me refined with riding coordinates:
 C65(H65A,H65B,H65C), C64(H64A,H64B,H64C)
8.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C55(H55), C13(H13), C15(H15), C23(H23), C25(H25), C45(H45),
 C43(H43), C62(H62), C55A(H55A), C53A(H53A), C43A(H43A), C45A(H45A)
8.d Fitted pentagon refined as free rotating group:
 N51(N52,C53,C54,C55), N42(N41,C45,C44,C43), N51A(C55A,C54A,C53A,N52A),
 N41A(N42A,C43A,C44A,C45A)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 498 electrons were 
found in a volume of 3022\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[C3H7NO] per Asymmetric Unit 
which account for 480 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              32593
_shelx_fab_checksum              94483
_olex2_submission_special_instructions 'No special instructions were received'