Carboxyl Position Directed Structure Diversity in Zirconium-Tricarboxylate Frameworks
Xia, Jun; Si, Jincheng; Zhou, Kang; Xia, Hai-Lun; Zhang, Jian; Xu, Yingqian; Wang, Lei; Liu, Xiao-Yuan; Dalton Transactions  (2023) –; doi:10.1039/D3DT03348A

data_7714461
_publ_section_title
;
 Carboxyl Position Directed Structure Diversity in
 Zirconium-Tricarboxylate Frameworks
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03348A
_journal_year                    2023
_chemical_formula_moiety         'C80 H51 N6 O35 S3 Zr6, 3(C2 H8 N)'
_chemical_formula_sum            'C86 H75 N9 O35 S3 Zr6'
_chemical_formula_weight         2438.05
_chemical_name_systematic        HIAM-4034
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-11 deposited with the CCDC.	2023-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   32.5504(6)
_cell_length_b                   32.5504(6)
_cell_length_c                   40.8188(13)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      57.207
_cell_measurement_theta_min      2.325
_cell_volume                     37454.5(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX4 V2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      193.15
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE Metaljet PHOTON II'
_diffrn_measurement_method       '\w and \f shutterless scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1097
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            96445
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.907
_diffrn_reflns_theta_min         3.730
_diffrn_source_current           2.86
_diffrn_source_power             0.1993134
_diffrn_source_voltage           69.69
_exptl_absorpt_coefficient_mu    2.515
_exptl_absorpt_correction_T_max  0.7224
_exptl_absorpt_correction_T_min  0.6594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1348 before and 0.0984 after correction.
The Ratio of minimum to maximum transmission is 0.9128.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.973
_exptl_crystal_description       block
_exptl_crystal_F_000             10998
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.608
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     733
_refine_ls_number_reflns         15232
_refine_ls_number_restraints     469
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0780P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1206
_refine_ls_wR_factor_ref         0.1336
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                11335
_reflns_number_total             15232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03348a2.cif
_cod_data_source_block           221231_wqangz_271159_1_0m_sq_sq
_cod_original_cell_volume        37454.4(18)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7714461
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.787
_shelx_estimated_absorpt_t_min   0.736
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(2)
 0.08(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(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,H) groups
3. Restrained distances
 N3-C39 = N4-C38
 1.4 with sigma of 0.01
 N6A-C50A = N6A-C49A
 1.45 with sigma of 0.01
 N5-C47 = N5-C48
 1.45 with sigma of 0.01
 N3-C40 = N4-C40
 1.45 with sigma of 0.01
 N6-C49 = N6-C50
 1.45 with sigma of 0.01
 C41-C40 = C45-C43
 1.5 with sigma of 0.01
 S2-C44 = S2-C41
 1.75 with sigma of 0.01
 O9-C45 = O10-C45
 1.25 with sigma of 0.01
 C42-C41 = C44-C43
 1.35 with sigma of 0.01
 C42-C43
 1.45 with sigma of 0.01
 C34-C31
 1.53 with sigma of 0.01
 C47-C48
 2.5 with sigma of 0.01
 C50A-C49A
 2.5 with sigma of 0.01
 C49-C50
 2.5 with sigma of 0.01
 C38-C40
 2.2 with sigma of 0.01
 C40-C39
 2.2 with sigma of 0.01
 N3-C40 \\sim N4-C40
 with sigma of 0.02
4. Restrained planarity
 S2, N3, C39, C38, C36, C41, C42, C34, C35, O10, O9, N4, C37, C40, C43, C45, C44
 with sigma of 0.1
 C28, C29, C30, C31, C32, C33, C38, C37, C36, C35, C34, C39
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C48 \\sim N5 \\sim C47: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
S2 \\sim O8 \\sim N3 \\sim C39 \\sim C38 \\sim C37 \\sim C36 \\sim C35 \\sim
C34 \\sim C41 \\sim C42 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim
C33 \\sim C27 \\sim O10 \\sim N4 \\sim C40 \\sim C43 \\sim C45 \\sim C44 \\sim
O9 \\sim O7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C49 \\sim N6 \\sim C50: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
C50A \\sim N6A \\sim C49A: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01 within 2A
Uanis(C48) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(S2) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(C39) \\sim
Ueq, Uanis(C38) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C36) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42)
\\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq,
Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C27)
\\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C43) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(O9)
\\sim Ueq, Uanis(O7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms
of 0.04
Uanis(N6A) \\sim Ueq, Uanis(C50A) \\sim Ueq, Uanis(C49A) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C49) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C50) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
6. Others
 Fixed Sof: S2(0.5) N3(0.5) C39(0.5) C38(0.5) C37(0.5) C36(0.5) H36(0.5)
 C35(0.5) H35(0.5) C34(0.5) C41(0.5) C42(0.5) H42(0.5) O10(0.5) O9(0.5) N4(0.5)
 H4A(0.5) C40(0.5) C43(0.5) C45(0.5) C44(0.5) H44(0.5) O19(0.5) H19A(0.5)
 H19B(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) N6(0.5) H6A(0.5) H6B(0.5)
 C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C50A(0.5) H50D(0.5) H50E(0.5) H50F(0.5)
 N6A(0.5) H6AA(0.5) H6AB(0.5) C49A(0.5) H49D(0.5) H49E(0.5) H49F(0.5) N5(0.5)
 H5A(0.5) H5B(0.5) C47(0.5) H47A(0.5) H47B(0.5) H47C(0.5) C48(0.5) H48A(0.5)
 H48B(0.5) H48C(0.5)
7.a Riding coordinates:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C)
7.b Rotating group:
 O17(H17A,H17B), O18(H18A,H18B), O19(H19A,H19B)
7.c Secondary CH2 refined with riding coordinates:
 N6(H6A,H6B), N6A(H6AA,H6AB), N5(H5A,H5B)
7.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C11(H11), C36(H36), C35(H35), C10(H10), C42(H42), C25(H25), C4(H4),
 C21(H21), C14(H14), C22(H22), C13(H13), C16(H16), C46(H46), C17(H17), C3(H3),
 C29(H29), C30(H30), C32(H32), C33(H33), C24(H24), N4(H4A), C44(H44)
7.e Fitted hexagon refined as free rotating group:
 C39(C38,C37,C36,C35,C34), C28(C29,C30,C31,C32,C33)
7.f Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C50A(H50D,H50E,H50F), C49A(H49D,
 H49E,H49F)
;
_shelx_res_checksum              73582
_shelx_fab_checksum              22065
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'