Amino group induced structural diversity and near-infrared emission of yttrium-tetracarboxylate frameworks
Xia, Hai-Lun; Zhou, Kang; Guo, Jiandong; Zhang, Jian; Huang, Xiaoxi; Luo, Dawei; Liu, Xiao-Yuan; Li, Jing; Chemical Science 13 (2022) 9321–9328; doi:10.1039/D2SC02683J

data_1567276
_publ_section_title
;
 Amino group induced structural diversity and near-infrared emission of
 yttrium-tetracarboxylate frameworks
;
_journal_issue                   32
_journal_name_full               'Chemical Science'
_journal_page_first              9321
_journal_page_last               9328
_journal_paper_doi               10.1039/D2SC02683J
_journal_volume                  13
_journal_year                    2022
_chemical_formula_moiety         'C232 H122 F16 N20 O48 S5 Y12'
_chemical_formula_sum            'C232 H122 F16 N20 O48 S5 Y12'
_chemical_formula_weight         5488.71
_space_group_crystal_system      orthorhombic
_space_group_IT_number           65
_space_group_name_Hall           '-C 2 2'
_space_group_name_H-M_alt        'C m m m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-02-10 deposited with the CCDC.	2022-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   40.568(2)
_cell_length_b                   41.959(2)
_cell_length_c                   19.6114(13)
_cell_measurement_reflns_used    9033
_cell_measurement_temperature    250.0
_cell_measurement_theta_max      66.703
_cell_measurement_theta_min      2.715
_cell_volume                     33382(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      250.0
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1039
_diffrn_reflns_av_unetI/netI     0.0758
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70779
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.426
_diffrn_reflns_theta_max         67.426
_diffrn_reflns_theta_min         2.715
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.746
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1580 before and 0.1048 after correction.
The Ratio of minimum to maximum transmission is 0.7351.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.546
_exptl_crystal_description       block
_exptl_crystal_F_000             5460
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         15675
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1105P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1711
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10612
_reflns_number_total             15675
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02683j2.cif
_cod_data_source_block           811_lxy_0m
_cod_depositor_comments
'Adding full bibliography for 1567276--1567277.cif.'
_cod_database_code               1567276
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.888
_shelx_estimated_absorpt_t_min   0.805
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H) groups
2. Restrained distances
 C20-C19
 1.39 with sigma of 0.02
 N1-H1
 0.96 with sigma of 0.02
 C20-C19 \\sim C21-C20 \\sim C21-C22 \\sim C21_$1-C22 \\sim C21_$1-C20_$1 \\sim
C20_$1-C19
 with sigma of 0.02
 S1-N2 \\sim S1-N7
 with sigma of 0.02
 N2-C17 \\sim N7-C16
 with sigma of 0.02
 C11-C13 \\sim C11-C17
 with sigma of 0.02
3. Restrained planarity
 S1, N2, N7, C11, C12, C13, C14, C15, C16, C17
 with sigma of 0.1
4. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2A
6. Others
 Fixed Sof: S1(0.25) S2(0.125) S3(0.125) S3A(0.125) O6(0.5) O6A(0.5) N2(0.25)
 N4(0.25) N6(0.25) N6A(0.25) N7(0.25) C12(0.25) C17(0.25) C16(0.25) C15(0.25)
 C14(0.25) H14(0.25) C13(0.25) H13(0.25) C27(0.25) C28(0.5) C41(0.5) C41A(0.5)
 C42(0.25) H42(0.25)
7.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C14(H14), C13(H13), C20(H20),
 C21(H21), C25(H25), C31(H31), C32(H32), C34(H34), C35(H35), C38(H38), C42(H42)
7.b Fitted hexagon refined as free rotating group:
 C12(C17,C16,C15,C14,C13)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20416
_shelx_fab_checksum              9265
_olex2_submission_special_instructions 'No special instructions were received'