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_7244710
_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         'C45 H48.5 Cu4 N3.5 O20, O'
_chemical_formula_sum            'C45 H48.5 Cu4 N3.5 O21'
_chemical_formula_weight         1228.53
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-11-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                73.768(2)
_cell_angle_beta                 71.193(4)
_cell_angle_gamma                87.559(4)
_cell_formula_units_Z            2
_cell_length_a                   14.6827(9)
_cell_length_b                   18.5378(5)
_cell_length_c                   21.3961(5)
_cell_measurement_reflns_used    16323
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      79.199
_cell_measurement_theta_min      3.803
_cell_volume                     5285.8(4)
_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)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device       'four-circle diffractometer'
_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  0.1045
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            69529
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.199
_diffrn_reflns_theta_min         3.803
_exptl_absorpt_coefficient_mu    1.247
_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    0.772
_exptl_crystal_description       plate
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   3.130
_exptl_transmission_factor_min   0.441
_refine_diff_density_max         1.783
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.482
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     725
_refine_ls_number_reflns         21813
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.481
_refine_ls_R_factor_all          0.1528
_refine_ls_R_factor_gt           0.1365
_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          0.3768
_refine_ls_wR_factor_ref         0.3896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16323
_reflns_number_total             21813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           6
_cod_original_formula_sum        'C45 H48.50 Cu4 N3.50 O21'
_cod_database_code               7244710
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O4B-C5
 1.28 with sigma of 0.001
 O3B-H3B = O4A-H4A
 0.82 with sigma of 0.004
 H4A-O3A
 2.4 with sigma of 0.004
 O4A-C5 = O3B-C5 = O3A-C5
 1.28 with sigma of 0.02
 O4B-H3B
 2.4 with sigma of 0.004
3. Restrained angles
 C5-O4A-H4A
 fixed at 109.5 with sigma of 0.02
 C5-O3B-H3B
 fixed at 109.5 with sigma of 0.02
4. Restrained planarity
 O3A, C5, O4A, H4A
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.0004
Uanis(O4B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O4A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(O3A) \\sim Ueq, Uanis(O3B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
6. Others
 Fixed Sof: N4(0.5) H4(0.5) H20A(0.5) H20B(0.5) O3A(0.4) O4A(0.4) O3B(0.6)
 O4B(0.6) O19(0.5) H19A(0.5) H19B(0.5) O22(0.5) O23(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) H45C(0.5) C46(0.5) H46A(0.5) H46B(0.5) H46C(0.5) H3B(0.6) H4A(0.4)
 O18(0.5) H18A(0.5) H18B(0.5)
7.a Rotating group:
 O17(H17A,H17B), O21(H21A,H21B), O18(H18A,H18B)
7.b Ternary CH refined with riding coordinates:
 N4(H4), N3(H3), C10(H10), C31(H31)
7.c Secondary CH2 refined with riding coordinates:
 O20(H20A,H20B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C30(H30A,H30B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), O19(H19A,H19B)
7.d Aromatic/amide H refined with riding coordinates:
 C3(H3A), C6(H6), C8(H8), C15(H15), C18(H18), C21(H21), C24(H24), C27(H27),
 C29(H29), C36(H36), C39(H39), C42(H42)
7.e Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C)
;
_shelx_res_checksum              80628
_shelx_fab_checksum              70262
_olex2_submission_special_instructions 'No special instructions were received'