Synthesis, solid-state, solution, and theoretical characterization of an “in-cage” scandium-NOTA complex
Aldrich, Kelly E.; Popov, Ivan A.; Root, Harrison D.; Batista, Enrique R.; Greer, Samuel M.; Kozimor, Stosh A.; Lilley, Laura M.; Livshits, Maksim Y.; Mocko, Veronika; Janicke, Michael T.; Scott, Brian L.; Stein, Benjamin W.; Yang, Ping; Dalton Transactions  (2022) –; doi:10.1039/D1DT03887G

data_7710593
_publ_section_title
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 Synthesis, solid-state, solution, and theoretical characterization of an
 &#x201C;in-cage&#x201D; scandium-NOTA complex
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03887G
_journal_year                    2022
_chemical_formula_moiety         'C28 H46 N6 Na3 O18 Sc2, H2 O, 10[H2O]'
_chemical_formula_sum            'C28 H70 N6 Na3 O30 Sc2'
_chemical_formula_weight         1129.79
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-04-28
_audit_creation_method
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Olex2 1.5-dev
(compiled 2022.04.21 svn.rca3783a0 for OlexSys, GUI svn.r6444)
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_audit_update_record
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2022-05-17 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 107.9050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.9608(7)
_cell_length_b                   19.7499(4)
_cell_length_c                   14.5059(3)
_cell_measurement_reflns_used    9872
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.40
_cell_volume                     9530.8(3)
_computing_cell_refinement       'APEX3 V.2018.7-2 (Bruker AXS, 2018)'
_computing_data_collection       'APEX3 V.2018.7-2 (Bruker AXS, 2018)'
_computing_data_reduction        'SAINT, v. 8.38A (Bruker AXS, 2013)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon II detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53239
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_min         2.042
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v. 2016/2 (Bruker AXS, 2016)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       plate
_exptl_crystal_F_000             4760
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         11371
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0314P)^2^+17.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0876
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9591
_reflns_number_total             11371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03887g2.cif
_cod_data_source_block           final_ccdc1
_cod_database_code               7710593
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.937
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 H18A-O18
 1 with sigma of 0.02
 O17-H17A
 1 with sigma of 0.02
 O19-H19A
 1 with sigma of 0.02
 H19B-O19
 0.95 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C18B) = Uanis(C17B)
Uanis(C26B) = Uanis(C25B) = Uanis(C21A) = Uanis(C18B) = Uanis(C17B)
4. Others
 Fixed Sof: C17A(0.75) H17C(0.75) H17D(0.75) C18A(0.75) H18C(0.75) H18D(0.75)
 C21A(0.75) H21A(0.75) H21B(0.75) C22A(0.75) H22A(0.75) H22B(0.75) C25A(0.75)
 H25A(0.75) H25B(0.75) C26A(0.75) H26A(0.75) H26B(0.75) C17B(0.25) H17E(0.25)
 H17F(0.25) C18B(0.25) H18E(0.25) H18F(0.25) C21B(0.25) H21C(0.25) H21D(0.25)
 C22B(0.25) H22C(0.25) H22D(0.25) C25B(0.25) H25C(0.25) H25D(0.25) C26B(0.25)
 H26C(0.25) H26D(0.25)
 Fixed Uiso: H18A(0.08) H17A(0.08) H18B(0.08) H17B(0.08) H19A(0.08) H19B(0.08)
5.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C16(H16A,H16B), C20(H20A,H20B),
  C24(H24A,H24B), C17A(H17C,H17D), C18A(H18C,H18D), C21A(H21A,H21B), C22A(H22A,
 H22B), C25A(H25A,H25B), C26A(H26A,H26B), C17B(H17E,H17F), C18B(H18E,H18F),
 C21B(H21C,H21D), C22B(H22C,H22D), C25B(H25C,H25D), C26B(H26C,H26D)
5.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 818 electrons were 
found in a volume of 2412\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 10[H2O] per Formula Unit 
which account for 800 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              25104
_shelx_hkl_checksum              54697
_shelx_fab_checksum              83557
_olex2_submission_special_instructions 'No special instructions were received'