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_7244707
_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
'C39 H39 Cd3 Cl N2 O21.5, 2(H2 O), C2 H2 N, 4(O), 0.25(C6 H14 N2 O2)'
_chemical_formula_sum            'C42.5 H48.5 Cd3 Cl N3.5 O28'
_chemical_formula_weight         1429.00
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-11-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_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                   20.7302(3)
_cell_length_b                   30.3248(3)
_cell_length_c                   17.7067(2)
_cell_measurement_reflns_used    12917
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      76.2490
_cell_measurement_theta_min      4.2260
_cell_volume                     11131.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0442
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            23003
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.838
_diffrn_reflns_theta_min         3.592
_exptl_absorpt_coefficient_mu    10.329
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             5704
_refine_diff_density_max         2.339
_refine_diff_density_min         -2.089
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     486
_refine_ls_number_reflns         5815
_refine_ls_number_restraints     113
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0767
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1458P)^2^+155.2447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2203
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5315
_reflns_number_total             5815
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00269h2.cif
_cod_data_source_block           9
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_formula_sum        'C42.50 H48.50 Cd3 Cl N3.50 O28'
_cod_database_code               7244707
_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, {H20A,H20B} of C20, {H11C,H11D} of C11, {H12C,H12D} of C12,
   {H10C,H10D} of C10, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, {H13A,H13B} of C16, All O(H,H) groups
2. Restrained distances
 O9-H9A = O9-H9B = O11-H11B = O11-H11A = O12-H12A = O12-H12B = O10-H10A = O10-
 H10B
 0.82 with sigma of 0.00001
 O13-H13A = O13-H13B
 0.82 with sigma of 0.0001
 O14-H14B = O14-H14A
 0.82 with sigma of 0.001
 N2-C24
 1.521 with sigma of 0.02
 N3-C22
 1.521 with sigma of 0.001
 O17-H14A
 1.761 with sigma of 0.04
 H12A-H12B
 1.4 with sigma of 0.02
 H13A-H13B
 1.42 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(C24) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(O18)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C23) \\sim Ueq,
Uanis(O17) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.001
Uanis(O6B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C16B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001
Uanis(C19A) \\sim Ueq, Uanis(C19B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.001
Uanis(O8A) \\sim Ueq, Uanis(O7B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.0001
4. Others
 Sof(O6A)=Sof(C19B)=Sof(O7B)=Sof(C16B)=Sof(O8A)=1-FVAR(1)
 Sof(C16A)=Sof(O8B)=Sof(O7A)=Sof(C19A)=Sof(O6B)=FVAR(1)
 Fixed Sof: H10A(0.5) H10B(0.5) H9A(0.5) H9B(0.5) H11A(0.5) H11B(0.5)
 O13(0.25) N2(0.5) H2A(0.5) H2B(0.5) O18(0.25) O16(0.5) O17(0.5) C21(0.25)
 H21(0.25) C23(0.25) H23A(0.25) H23B(0.25) H23C(0.25) N3(0.25) C22(0.25)
 H22A(0.25) H22B(0.25) H22C(0.25) H13A(0.25) H13B(0.25)
5.a Ternary CH refined with riding coordinates:
 N1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C11(H11C,H11D), C20(H20A,H20B), C10(H10C,H10D), C12(H12C,H12D), N2(H2A,H2B)
5.c Me refined with riding coordinates:
 C23(H23A,H23B,H23C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C8(H8), C14(H14), C21(H21), C17(H17), C16(H16)
5.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
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_shelx_res_checksum              13292
_olex2_submission_special_instructions 'No special instructions were received'