Highly Connected Framework Materials from Flexible Tetra-Isophthalate Ligands
Chahine, Ali; Chaffee, Alan L.; Knowles, Gregory P.; Turner, David Roger; Batten, Stuart R.; CrystEngComm  (2022) –; doi:10.1039/D2CE00269H

data_7244702
_publ_section_title
;
 Highly Connected Framework Materials from Flexible Tetra-Isophthalate
 Ligands
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00269H
_journal_year                    2022
_chemical_formula_moiety         'C38 H32 Cu2 N2 O18'
_chemical_formula_sum            'C38 H32 Cu2 N2 O18'
_chemical_formula_weight         931.73
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.670(4)
_cell_length_b                   26.670(4)
_cell_length_c                   25.930(5)
_cell_measurement_reflns_used    18885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.372
_cell_measurement_theta_min      1.095
_cell_volume                     18444(5)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.710919
_diffrn_reflns_av_R_equivalents  0.2795
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            646497
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.095
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.671
_exptl_crystal_description       plate
_exptl_crystal_F_000             3808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.4342
_exptl_transmission_factor_min   0.2736
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.036
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.502(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         18885
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      2.219
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0367
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0616P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1089
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                12219
_reflns_number_total             18885
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           1
_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_cell_volume        18444(6)
_cod_database_code               7244702
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.498(12)
 0.502(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups, H3 of O3, H10 of O10, H14 of O14
3. Restrained distances
 O18-H18A = O18-H18B
 0.82 with sigma of 0.001
 O10_$3-H10
 1.673 with sigma of 0.02
 H14_$3-O7_$4
 1.644 with sigma of 0.04
4. Restrained planarity
 O7, H7, O8, C14
 with sigma of 0.1
 H3, O3, C7, O4
 with sigma of 0.1
 C25, O9, O10, H10
 with sigma of 0.1
 O13, C34, O14, H14
 with sigma of 0.1
 O14_$1, H14_$1, H7, O7
 with sigma of 0.1
5. Others
 Fixed Sof: H3(0.5) H7(0.5) H10(0.5) H14(0.5)
6.a Rotating group:
 O17(H17A,H17B), O18(H18A,H18B)
6.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
6.c Secondary CH2 refined with riding coordinates:
 C9(H9B,H9A), C10(H10B,H10A), C19(H19A,H19B), C20(H20A,H20B), C21(H21B,H21A),
 C30(H30A,H30B)
6.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C8(H8), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26),
 C29(H29), C32(H32), C35(H35), C38(H38)
6.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7), O10(H10), O14(H14)
;
_shelx_res_checksum              29154
_shelx_fab_checksum              51340
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'