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_7244713
_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 H25 Cu3.5 N2 O19'
_chemical_formula_sum            'C38 H25 Cu3.5 N2 O19'
_chemical_formula_weight         1035.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-12-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.93(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.731(5)
_cell_length_b                   26.455(5)
_cell_length_c                   26.552(5)
_cell_measurement_reflns_used    2593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.382
_cell_measurement_theta_min      0.839
_cell_volume                     16521(7)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'MX2 Synchotron'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.710877
_diffrn_reflns_av_R_equivalents  0.1804
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28290
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        16.382
_diffrn_reflns_theta_max         16.382
_diffrn_reflns_theta_min         0.839
_diffrn_source                   'MX2 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    0.833
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             4164
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   0.4349
_exptl_transmission_factor_min   0.1219
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.427
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4433
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.446
_refine_ls_R_factor_all          0.1713
_refine_ls_R_factor_gt           0.1391
_refine_ls_shift/su_max          0.000
_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          0.3889
_refine_ls_wR_factor_ref         0.4252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2593
_reflns_number_total             4433
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           2
_cod_original_formula_sum        'C38 H25 Cu3.50 N2 O19'
_cod_database_code               7244713
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.913
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 C2-C1 = C7-C6 = C15-C14 = C18-C17 = C21-C20 = C26-C25 = C34-C33 = C37-C36
 1.502 with sigma of 0.001
3. Restrained planarity
 O15, O16, C36, C37
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(Cu2) \\sim Ueq, Uanis(Cu1) \\sim Ueq, Uanis(Cu3) \\sim Ueq, Uanis(Cu4)
\\sim Ueq, Uanis(Cu6) \\sim Ueq, Uanis(Cu5) \\sim Ueq, : with sigma of 0.01 and
sigma for terminal atoms of 0.001
: with sigma of 0.01 and sigma for terminal atoms of 0.001
5. Others
 Fixed Sof: O15(0.5) O16(0.5) H1(0.5) H2(0.5)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
6.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C28(H28A,H28B), C29(H29A,H29B),
 C30(H30A,H30B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C16(H16), C13(H13), C19(H19), C22(H22), C24(H24),
 C27(H27), C38(H38), C35(H35), C32(H32)
6.d Fitted hexagon refined as free rotating group:
 C17(C16,C14,C13,C12,C19), C38(C36,C35,C33,C32,C31)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              21463
_shelx_fab_checksum              79437
_olex2_submission_special_instructions 'No special instructions were received'