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_7244700
_publ_section_title
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 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         'C40 H28.733 Cu2.4 N2 O16.8, C4 H16 N2'
_chemical_formula_sum            'C44 H44.73 Cu2.4 N4 O16.8'
_chemical_formula_weight         1050.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           53
_space_group_name_Hall           '-P 2ac 2'
_space_group_name_H-M_alt        'P m n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_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            12
_cell_length_a                   42.6882(13)
_cell_length_b                   14.5716(6)
_cell_length_c                   26.9781(12)
_cell_measurement_reflns_used    8453
_cell_measurement_temperature    122.99(11)
_cell_measurement_theta_max      76.842
_cell_measurement_theta_min      3.276
_cell_volume                     16781.3(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      122.99(11)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1462
_diffrn_reflns_av_unetI/netI     0.0796
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -53
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            83977
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.842
_diffrn_reflns_theta_min         3.276
_exptl_absorpt_coefficient_mu    1.638
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34061
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       plate
_exptl_crystal_F_000             6489
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   1.00000
_exptl_transmission_factor_min   0.34061
_refine_diff_density_max         3.394
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.488
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1025
_refine_ls_number_reflns         17485
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.488
_refine_ls_R_factor_all          0.2532
_refine_ls_R_factor_gt           0.1797
_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          0.4363
_refine_ls_wR_factor_ref         0.4904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8453
_reflns_number_total             17485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           4
_cod_original_formula_sum        'C44 H44.73 Cu2.40 N4 O16.80'
_cod_database_code               7244700
_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, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C42-C41
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C49A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C44B) \\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(C49A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Cu5A(0.75) O26(0.75) H2(0.6) H1(0.6) C53(0.5) H53A(0.5) H53B(0.5)
 C52(0.5) H52A(0.5) H52B(0.5) C51(0.5) H51A(0.5) H51B(0.5) C50(0.5) H50A(0.5)
 H50B(0.5) H43(0.5) H43A(0.5) C45A(0.5) H45A(0.5) C56A(0.5) H56A(0.5) C55A(0.5)
 C62A(0.5) H62A(0.5) C54A(0.5) H54A(0.5) H54B(0.5) C49A(0.5) H49A(0.5)
 H49B(0.5) Cu2A(0.45) O25(0.45) H25A(0.9) C56B(0.5) H56B(0.5) C55B(0.5)
 C62B(0.5) H62B(0.5) C49B(0.5) H49C(0.5) H49D(0.5) H8A(0.5) H8B(0.5) H69B(0.5)
 H69C(0.5) H70A(0.5) H70B(0.5) H70C(0.5) H6A(0.5) H6B(0.5) H63A(0.5) H63B(0.5)
 H63C(0.5) H64A(0.5) H64B(0.5) H64C(0.5) Cu5B(0.125) Cu2B(0.025) C45B(0.5)
 H45B(0.5) C44A(0.5) C44B(0.5)
5.a Ternary CH refined with riding coordinates:
 N2(H2), N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B),
 C22(H22A,H22B), C23(H23A,H23B), C32(H32A,H32B), C53(H53A,H53B), C52(H52A,H52B),
  C51(H51A,H51B), C50(H50A,H50B), C54A(H54A,H54B), C49A(H49A,H49B), C49B(H49C,
 H49D), N8(H8A,H8B), N6(H6A,H6B), N5(H5A,H5B), N7(H7A,H7B)
5.c Me refined with riding coordinates:
 C69(H69A,H69B,H69C)
5.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C3(H3), C5(H5), C12(H12), C15(H15), C18(H18), C25(H25), C28(H28),
 C31(H31), C34(H34), C37(H37), C40(H40), C59(H59), C43(H43), C43(H43A),
 C48(H48), C45A(H45A), C56A(H56A), C62A(H62A), C56B(H56B), C62B(H62B),
 C45B(H45B)
5.e Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,
 H65C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C)
5.f Idealised tetrahedral OH refined as rotating group:
 O25(H25A)
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_shelx_res_checksum              12631
_shelx_fab_checksum              60012
_olex2_submission_special_instructions 'No special instructions were received'