Design, Isolation, and Spectroscopic Analysis of a Tetravalent Terbium Complex.
Rice, Natalie T.; Popov, Ivan A.; Russo, Dominic R.; Bacsa, John; Batista, Enrique R.; Yang, Ping; Telser, Joshua; La Pierre, Henry S.; Journal of the American Chemical Society 141 (2019) 13222–13233; doi:10.1021/jacs.9b06622

data_4127825
_publ_section_title
;
 Design, Isolation, and Spectroscopic Analysis of a Tetravalent Terbium
 Complex.
;
_journal_issue                   33
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13222
_journal_page_last               13233
_journal_paper_doi               10.1021/jacs.9b06622
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C60 H138 K N16 O P4 Tb'
_chemical_formula_sum            'C60 H138 K N16 O P4 Tb'
_chemical_formula_weight         1421.76
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-10
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.512(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4833(11)
_cell_length_b                   15.9381(8)
_cell_length_c                   25.5112(16)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.975
_cell_measurement_theta_min      2.70
_cell_volume                     8317.8(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0572
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            79238
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.334
_diffrn_reflns_theta_min         2.702
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6696
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1889 before and 0.0893 after correction. The Ratio of minimum to maximum transmission is 0.9121. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       prism
_exptl_crystal_F_000             3048
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by ---'
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.324
_refine_diff_density_max         1.260
_refine_diff_density_min         -1.283
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         20139
_refine_ls_number_restraints     370
_refine_ls_restrained_S_all      2.392
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0447P)^2^+0.9753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0863
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17841
_reflns_number_total             20139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06622_si_005.cif
_cod_data_source_block           ntr-03-018_180k_l
_cod_database_code               4127825
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
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
 O1_3-C2_3
 1.425 with sigma of 0.003
 O1_3-C1_3
 1.425 with sigma of 0.003
 C1_3-C2_3
 1.512 with sigma of 0.005
 C3_3-C4_3
 1.512 with sigma of 0.005
 C1_3-C3_3
 2.406 with sigma of 0.004
 C2_3-O1_3
 2.467 with sigma of 0.004
 C4_3-O1_3
 2.467 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O1_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C2_3) = Uanis(C3_3)
4. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 P1_1, N1_1, N2_1, N3_1, N4_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
 C9_1, C10_1, C11_1, C12_1, C13_1, C14_1
 P1_2, N1_2, N2_2, N3_2, N4_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2,
 C9_2, C10_2, C11_2, C12_2, C13_2, C14_2
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.004
 O1_3, C1_3, C2_3, C3_3, C4_3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Same fragment restrains
{P1_2, N1_2, N2_2, N3_2, N4_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2,
C9_2, C10_2, C11_2, C12_2, C13_2, C14_2}
as
{P1_1, N1_1, N2_1, N3_1, N4_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1,
C9_1, C10_1, C11_1, C12_1, C13_1, C14_1} sigma for 1-2: 0.002 1-3: 0.004
6. Others
 Fixed Sof: O1(0.5) C1(0.5) H1A(0.5) H1B(0.5) C2(0.5) H2A(0.5) H2B(0.5)
 H2C(0.5) C3(0.5) H3A(0.5) H3B(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
7.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C12(H12A,H12B), C13(H13A,H13B), C1(H1A,H1B), C2(H2A,
 H2B), C12(H12A,H12B), C13(H13A,H13B), C1(H1A,H1B), C3(H3A,H3B)
7.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,
 H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C),
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,
 H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C2(H2A,
 H2B,H2C), C4(H4A,H4B,H4C)
;
_smtbx_masks_void_probe_radius   0.3
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9714
_shelx_hkl_checksum              4030
_shelx_fab_checksum              39612
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'The crystal was mounted on a None'
_olex2_submission_original_sample_id NTR-03-018_180K
_olex2_submission_special_instructions 'No special instructions were received'