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_7244706
_publ_section_title
;
 Highly Connected Framework Materials from Flexible Tetra-Isophthalate
 Ligands
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_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00269H
_journal_year                    2022
_chemical_formula_moiety         'C42 H33 Cu3 N2 O19, C3 H7 N O, 2.25(O)'
_chemical_formula_sum            'C45 H40 Cu3 N3 O22.25'
_chemical_formula_weight         1169.42
_space_group_crystal_system      orthorhombic
_space_group_IT_number           63
_space_group_name_Hall           '-C 2c 2'
_space_group_name_H-M_alt        'C m c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
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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                   29.643(6)
_cell_length_b                   18.639(4)
_cell_length_c                   27.125(5)
_cell_measurement_reflns_used    5851
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.377
_cell_measurement_theta_min      1.291
_cell_volume                     14987(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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_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     0.710919
_diffrn_reflns_av_R_equivalents  0.0854
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            99844
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.377
_diffrn_reflns_theta_min         1.291
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       block
_exptl_crystal_F_000             4768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7463
_exptl_transmission_factor_min   0.4478
_refine_diff_density_max         1.933
_refine_diff_density_min         -1.380
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         7972
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0746
_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^)+(0.1505P)^2^+49.8177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2286
_refine_ls_wR_factor_ref         0.2501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5851
_reflns_number_total             7972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           5
_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_database_code               7244706
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
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1. 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, All O(H) groups
2. Restrained distances
 O6A-C17
 1.26 with sigma of 0.02
 O5B-C17
 1.26 with sigma of 0.01
 O12_$2-H11
 1.882 with sigma of 0.02
 H10_$1-H10
 1.415 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O5B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
Uanis(C22) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O6A) \\sim Ueq: with sigma of 0.0001 and sigma for terminal atoms of
0.0002
4. Others
 Fixed Sof: H9(0.5) H10(0.5) H11(0.5) O5A(0.75) O6A(0.75) O5B(0.25) O6B(0.25)
 O12(0.5) N2(0.5) C22(0.5) H22(0.5) C23(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) O13(0.25) O14(0.25) O16(0.125)
5.a Ternary CH refined with riding coordinates:
 C10(H10A)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B)
5.c Me refined with riding coordinates:
 C24(H24A,H24B,H24C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C15(H15), C18(H18), C21(H21), C22(H22)
5.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C)
5.f Idealised tetrahedral OH refined as rotating group:
 O9(H9), O10(H10), O11(H11)
;
_shelx_res_checksum              42419
_shelx_fab_checksum              36856
_olex2_submission_special_instructions 'No special instructions were received'