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_1567277
_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         'C47.453 H23.453 F4 N3 O12.905 S Y3'
_chemical_formula_sum            'C47.48 H22.51 F4 N3 O12.97 S Y3'
_chemical_formula_weight         1217.37
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2022-04-08 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            4
_cell_length_a                   21.358(10)
_cell_length_b                   35.038(16)
_cell_length_c                   20.494(9)
_cell_measurement_reflns_used    5980
_cell_measurement_temperature    173.00
_cell_measurement_theta_max      47.019
_cell_measurement_theta_min      2.809
_cell_volume                     15337(12)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 V2019.11-0 (Bruker, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 7.41
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'nylon loop'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1519
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            47876
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.906
_diffrn_reflns_theta_min         2.108
_diffrn_source_current           2.86
_diffrn_source_power             0.1993706
_diffrn_source_voltage           69.71
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.230
_exptl_absorpt_correction_T_max  0.7512
_exptl_absorpt_correction_T_min  0.5209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1733 before and 0.0761 after correction.
The Ratio of minimum to maximum transmission is 0.6934.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    0.527
_exptl_crystal_description       block
_exptl_crystal_F_000             2405
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00110(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   0.922
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1227
_refine_ls_R_factor_gt           0.0853
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1570P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3686
_reflns_number_total             7538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02683j2.cif
_cod_data_source_block           a2
_cod_depositor_comments
'Adding full bibliography for 1567276--1567277.cif.'
_cod_database_code               1567277
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.887
_shelx_estimated_absorpt_t_min   0.866
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Restrained distances
 O5A-C14 = O5B-C7 = O8-C7
 1.25 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
S1 \\sim N2 \\sim C11 \\sim C12 \\sim C13: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
O5B \\sim C14: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O8 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(O8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(S1) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms
of 0.02
Uanis(O5B) \\sim Ueq, Uanis(C14) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(O5A) = Uanis(C14)
Uanis(O5B) = Uanis(C7) = Uanis(O8)
4. Others
 Sof(O5B)=Sof(O8)=Sof(C7)=Sof(H7)=0.5*(1-FVAR(2))
 Sof(C14)=Sof(H14)=0.25*FVAR(2)
 Sof(O5A)=0.5*FVAR(2)
 Fixed Sof: S1(0.25) N1(0.25) H1A(0.25) H1B(0.25) N2(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C14(H14), C15(H15)
5.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15391
_shelx_fab_checksum              28682
_olex2_submission_special_instructions 'No special instructions were received'