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_7710592
_publ_section_title
;
 Synthesis, solid-state, solution, and theoretical characterization of an
 &#x201C;in-cage&#x201D; scandium-NOTA complex
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03887G
_journal_year                    2022
_chemical_formula_moiety
'C28.01 H45.37 N6 Na3 O18 Sc2, 5.5(H2 O), 3.5(O), 0.5(H2 O2)'
_chemical_formula_sum            'C28.01 H59.39 N6 Na3 O28 Sc2'
_chemical_formula_weight         1087.16
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-08 deposited with the CCDC.	2022-05-20 downloaded from the CCDC.
;
_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(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.40
_cell_volume                     9530.8(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.407
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0684 before and 0.0508 after correction. The Ratio of minimum to maximum transmission is 0.9468. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       plate
_exptl_crystal_F_000             4547
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.781
_refine_diff_density_min         -0.765
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         11371
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0668P)^2^+46.0106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1583
_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
_cod_database_code               7710592
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.938
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 H18C-O18
 0.92 with sigma of 0.02
 H18D-O18
 0.92 with sigma of 0.02
 H28E-O28 = O28-H28D
 0.96 with sigma of 0.02
 O24-H24C = H24C-H24D
 0.96 with sigma of 0.02
 H24D-H24C
 1.45 with sigma of 0.02
 H27A-O27 = O27-H27B
 0.96 with sigma of 0.02
 H22E-O22 = O22-H22F
 0.96 with sigma of 0.02
 H31B-O31 = O31-H31A
 0.96 with sigma of 0.02
 H32A-O32 = O32-H32B
 0.96 with sigma of 0.02
 H21E-O20 = O20-H21F
 0.96 with sigma of 0.02
3. Rigid bond restraints
 O24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O26
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C22A \\sim C21A \\sim C18A \\sim C26B \\sim C25B: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
C26A \\sim C25A \\sim C22B \\sim C21B \\sim C18B \\sim C17B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
O23 \\sim O24: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O32 \\sim O31: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O30 \\sim O29: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C17B) = Uanis(C18B) = Uanis(C21B) = Uanis(C22B) = Uanis(C25A) =
Uanis(C26A)
Uanis(C21A) = Uanis(C22A) = Uanis(C25B) = Uanis(C26B) = Uanis(C18A) =
Uanis(C17A)
Uanis(O32) = Uanis(O31)
Uanis(O29) = Uanis(O30)
Uanis(O21) = Uanis(O20)
5. Others
 Fixed Sof: C26B(0.75) H26A(0.75) H26B(0.75) C22A(0.75) H22A(0.75) H22B(0.75)
 C25B(0.75) H25A(0.75) H25B(0.75) C18A(0.75) H18A(0.75) H18B(0.75) C17A(0.75)
 H17A(0.75) H17B(0.75) C26A(0.25) H26C(0.25) H26D(0.25) C22B(0.25) H22C(0.25)
 H22D(0.25) C21B(0.25) H21C(0.25) H21D(0.25) C17B(0.25) H17E(0.25) C25A(0.25)
 H25C(0.25) C18B(0.25) H18E(0.25) H18F(0.25) O32(0.5) H32B(0.5) H32A(0.5)
 O26(0.5) O21(0.5) O22(0.5) H22E(0.5) H22F(0.5) O29(0.75) O23(0.5) O31(0.5)
 H31A(0.5) H31B(0.5) O30(0.25) O20(0.5) H21E(0.5) H21F(0.5) O0AA(0.5)
 Fixed X: Sc2(0.32969) Sc1(0.36149) O1(0.30523) O2(0.25803) O5(0.321771)
 O14(0.314409) O3(0.37804) O12(0.318161) O7(0.33262) O11(0.30978) O8(0.38934)
 O6(0.317321) O13(0.315141) O9(0.29429) O16(0.318061) O15(0.26486) O10(0.28908)
 O4(0.42567) N1(0.35906) N3(0.38695) N2(0.4296) N5(0.383201) N4(0.37597)
 C1(0.29154) N6(0.387409) C10(0.37579) H10A(0.374929) H10B(0.39495) C8(0.43094)
 H8A(0.44226) H8B(0.435889) C11(0.363261) H11A(0.37119) H11B(0.33568)
 C26B(0.41133) H26A(0.416699) H26B(0.433749) C3(0.39177) H3A(0.39501)
 H3B(0.384429) C4(0.432039) H4A(0.451489) H4B(0.443549) C21A(0.406528)
 H21A(0.38843) H21B(0.42775) C22A(0.4206) H22A(0.42862) H22B(0.44018)
 C25B(0.402559) C16(0.35402) C14(0.362) C18A(0.407009) C20(0.36447)
 C6(0.445789) C5(0.414579) C28(0.25433) C24(0.36989) C17A(0.38799)
 H17A(0.363501) H17B(0.40831) C15(0.308941) C27(0.279929) C23(0.33012)
 C13(0.361131) C19(0.328171) C12(0.36746) C2(0.3197) C7(0.452) C9(0.33474)
 Na2(0.23129) Na3(0.247429) O18(0.246089) O17(0.236059) Na1(0.30666)
 C26A(0.393981) C22B(0.4078) C21B(0.421081) C17B(0.410769) C25A(0.41225)
 C18B(0.39865) O19(0.22062) O27(0.07886) O24(0.03039) O32(0.03189) O28(0.16606)
 O26(0.02282) O21(0.04772) O25(0.00718) O22(0.032109) O29(-0.03773) O23(-
 0.003421) O31(0.03098) O30(-0.04096) O20(0.05991) H18C(0.2713) H18D(0.230549)
 H17D(0.25996)
 Fixed Y: Sc2(0.58162) Sc1(0.839469) O1(0.796679) O2(0.764649) O5(0.919519)
 O14(0.61141) O3(0.734019) O12(0.64052) O7(0.80211) O11(0.59356) O8(0.858251)
 O6(1.02274) O13(0.562341) O9(0.492) O16(0.688141) O15(0.623281) O10(0.379649)
 O4(0.659961) N1(0.833981) N3(0.945889) N2(0.825861) N5(0.627021) N4(0.49095)
 C1(0.78731) N6(0.601861) C10(0.996229) H10A(1.044539) H10B(0.994479)
 C8(0.94874) H8A(0.989009) H8B(0.94632) C11(0.95879) H11A(0.9991)
 H11B(0.962429) C26B(0.489149) H26A(0.444059) H26B(0.509459) C3(0.784989)
 H3A(0.78116) H3B(0.7411) C4(0.80604) H4A(0.76967) H4B(0.84506) C21A(0.67595)
 H21A(0.714109) H21B(0.69462) C22A(0.63989) H22A(0.671721) H22B(0.610061)
 C25B(0.52957) C16(0.42585) C14(0.833549) C18A(0.57488) C20(0.668322)
 C6(0.77132) C5(0.716209) C28(0.74037) C24(0.633941) C17A(0.50482)
 H17A(0.49982) H17B(0.469419) C15(0.432619) C27(0.68097) C23(0.60023)
 C13(0.83029) C19(0.63113) C12(0.90175) C2(0.80585) C7(0.88991) C9(0.979508)
 Na2(0.34782) Na3(0.522281) O18(0.409789) O17(0.55867) Na1(0.297689)
 C26A(0.49099) C22B(0.67191) C21B(0.648061) C17B(0.49858) C25A(0.55933)
 C18B(0.549449) O19(0.4252) O27(0.33873) O24(0.1372) O32(0.35293) O28(0.34487)
 O26(0.24094) O21(0.41938) O25(0.02013) O22(0.26523) O29(0.45821) O23(0.11985)
 O31(0.368461) O30(0.42865) O20(0.447049) H18C(0.398391) H18D(0.41166)
 H17D(0.57342)
 Fixed Z: Sc2(0.49933) Sc1(0.08919) O1(0.01203) O2(-0.123011) O5(0.103331)
 O14(0.207669) O3(0.11609) O12(0.770599) O7(0.20892) O11(0.62541) O8(0.24591)
 O6(0.162061) O13(0.34589) O9(0.484109) O16(0.46175) O15(0.430309) O10(0.49331)
 O4(0.1926) N1(-0.076719) N3(0.05436) N2(0.0948) N5(0.627251) N4(0.55081) C1(-
 0.080571) N6(0.442479) C10(0.11703) H10A(0.093881) H10B(0.17993) C8(0.06805)
 H8A(0.098381) H8B(0.00912) C11(-0.04841) H11A(-0.0708) H11B(-0.050811)
 C26B(0.51901) H26A(0.50684) H26B(0.57193) C3(-0.073931) H3A(-0.13769) H3B(-
 0.057491) C4(-0.003281) H4A(0.004569) H4B(-0.03107) C21A(0.58202)
 H21A(0.551991) H21B(0.635341) C22A(0.506409) H22A(0.46632) H22B(0.53206)
 C25B(0.42662) C16(0.53216) C14(0.37568) C18A(0.68491) C20(0.686399)
 C6(0.165481) C5(0.157201) C28(0.38271) C24(0.3469) C17A(0.660821)
 H17A(0.676489) H17B(0.688641) C15(0.5021) C27(0.42773) C23(0.29492)
 C13(0.27193) C19(0.69758) C12(-0.11422) C2(-0.13756) C7(0.12983) C9(0.128141)
 Na2(0.3835) Na3(0.325261) O18(0.266049) O17(0.16073) Na1(0.612321)
 C26A(0.45392) C22B(0.51419) C21B(0.61863) C17B(0.6308) C25A(0.44278)
 C18B(0.691971) O19(0.064361) O27(0.80733) O24(0.55604) O32(0.938439)
 O28(0.893801) O26(0.67989) O21(0.10772) O25(0.65719) O22(0.08682) O29(0.83131)
 O23(0.34873) O31(0.95039) O30(0.84343) O20(0.12693) H18C(0.2643)
 H18D(0.202909) H17D(0.167981)
6.a Free rotating group:
 O19(H19A,H19B), O27(H27A,H27B), O24(H24C,H24D), O32(H32B,H32A), O28(H28D,
 H28E), O22(H22E,H22F), O31(H31A,H31B), O20(H21E,H21F)
6.b Rotating group:
 O17(H17C)
6.c Secondary CH2 refined with riding coordinates:
 C25B(H25A,H25B), C16(H16A,H16B), C18A(H18A,H18B), C20(H20A,H20B), C6(H6A,H6B),
  C24(H24A,H24B), C12(H12A,H12B), C2(H2A,H2B), C7(H7A,H7B), C26A(H26C,H26D),
 C22B(H22C,H22D), C21B(H21C,H21D), C18B(H18E,H18F)
6.d Aromatic/amide H refined with riding coordinates:
 C17B(H17E), C25A(H25C)
6.e Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              87207
_shelx_hkl_checksum              54697
_olex2_submission_special_instructions 'No special instructions were received'