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_4127826
_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_absolute_configuration ad
_chemical_formula_moiety         'C64 H129 K N16 O P4 Tb'
_chemical_formula_sum            'C64 H129 K N16 O P4 Tb'
_chemical_formula_weight         1460.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-07
_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                 108.768(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.279(5)
_cell_length_b                   14.385(3)
_cell_length_c                   23.002(5)
_cell_measurement_reflns_used    9377
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.71
_cell_volume                     7606(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2016)'
_computing_data_collection       'APEX2 v2016.5-1 (Bruker, 2014)'
_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(2)
_diffrn_detector_area_resol_mean 7.495
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            96071
_diffrn_reflns_point_group_measured_fraction_full 0.884
_diffrn_reflns_point_group_measured_fraction_max 0.806
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.640
_diffrn_reflns_theta_min         2.285
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_T_max  0.4942
_exptl_absorpt_correction_T_min  0.3585
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1382 before and 0.0870 after correction. The Ratio of minimum to maximum transmission is 0.7254. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.276
_exptl_crystal_description       prism
_exptl_crystal_F_000             3108
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.203
_refine_diff_density_max         1.057
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.124
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.018(11)
_refine_ls_extinction_coef       0.00035(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         20674
_refine_ls_number_restraints     607
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0362P)^2^+30.3923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1097
_refine_ls_wR_factor_ref         0.1283
_reflns_Friedel_coverage         0.633
_reflns_Friedel_fraction_full    0.777
_reflns_Friedel_fraction_max     0.626
_reflns_number_gt                15164
_reflns_number_total             20674
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06622_si_002.cif
_cod_data_source_block           ntr-03-057_l
_cod_database_code               4127826
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.982(11)
 0.018(11)
2. 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
3. Rigid body (RIGU) restrains
 P2, N7, N8, C34, C31, C33, C27, C25, N9, C32, C20, C26, C28, C35, C23, C29,
 C24, C21, C22, N6
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 P3, N10, N11, C39, N12, C49, C42, C46, C43, C38, C36, C41, C37, C45, C47, C50,
  C48, C40, C44, N1
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 C56, C60, C59, C57, C58, N15, P4, N14, N16, C64, C61, C51, C55, C54, C53, C52,
  C65, C63, C62, N13
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 P1, N3, N4, N2, N5, C15, C19, C7, C8, C6, C10, C16, C5, C14, C13, C11, C9,
 C18, C12, C17
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 C2, C1, O1, C3, C4
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
4.a Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C34(H34A,H34B), C15(H15A,H15B), C19(H19A,H19B), C49(H49A,
 H49B), C42(H42A,H42B), C46(H46A,H46B), C64(H64A,H64B), C43(H43A,H43B), C7(H7A,
 H7B), C61(H61A,H61B), C38(H38A,H38B), C41(H41A,H41B), C31(H31A,H31B), C37(H37A,
 H37B), C33(H33A,H33B), C56(H56A,H56B), C45(H45A,H45B), C8(H8A,H8B), C60(H60A,
 H60B), C27(H27A,H27B), C47(H47A,H47B), C6(H6A,H6B), C10(H10A,H10B), C25(H25A,
 H25B), C32(H32A,H32B), C16(H16A,H16B), C5(H5A,H5B), C20(H20A,H20B), C51(H51A,
 H51B), C26(H26A,H26B), C55(H55A,H55B), C59(H59A,H59B), C54(H54A,H54B),
 C28(H28A,H28B), C14(H14A,H14B), C40(H40A,H40B), C57(H57A,H57B), C53(H53A,H53B),
  C13(H13A,H13B), C1(H1A,H1B), C35(H35A,H35B), C11(H11A,H11B), C44(H44A,H44B),
 C9(H9A,H9B), C52(H52A,H52B), C23(H23A,H23B), C29(H29A,H29B), C24(H24A,H24B),
 C50(H50A,H50B), C65(H65A,H65B), C63(H63A,H63B), C18(H18A,H18B), C21(H21A,H21B),
  C58(H58A,H58B), C48(H48A,H48B), C62(H62A,H62B), C12(H12A,H12B), C22(H22A,
 H22B), C17(H17A,H17B), C3(H3A,H3B)
4.b Aromatic/amide H refined with riding coordinates:
 C36(H36)
4.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              11839
_shelx_hkl_checksum              39803
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id NTR-03-057
_olex2_submission_special_instructions 'No special instructions were received'