Molecular Complex of Tb in the +4 Oxidation State.
Palumbo, Chad T.; Zivkovic, Ivica; Scopelliti, Rosario; Mazzanti, Marinella; Journal of the American Chemical Society 141 (2019) 9827–9831; doi:10.1021/jacs.9b05337

data_4128279
_publ_section_title
;
 Molecular Complex of Tb in the +4 Oxidation State.
;
_journal_issue                   25
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9827
_journal_page_last               9831
_journal_paper_doi               10.1021/jacs.9b05337
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C48 H108 O16 Si4 Tb'
_chemical_formula_sum            'C48 H108 O16 Si4 Tb'
_chemical_formula_weight         1212.62
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.4478(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.0696(5)
_cell_length_b                   13.4628(2)
_cell_length_c                   40.7459(8)
_cell_measurement_reflns_used    14952
_cell_measurement_temperature    140.00(10)
_cell_measurement_theta_max      73.0670
_cell_measurement_theta_min      3.8360
_cell_volume                     13120.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      140.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2665
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -113.00 -19.00   1.00    7.50    --  -43.01 -57.00 -90.00   94
  2  \w   -123.00 -94.00   1.00    7.50    --  -43.01 -99.00  60.00   29
  3  \w    -66.00  28.00   1.00    7.50    --  -43.01  57.00  60.00   94
  4  \w   -124.00 -81.00   1.00    7.50    --  -43.01 -99.00   0.00   43
  5  \w    -87.00 -27.00   1.00    7.50    --  -43.01 125.00 120.00   60
  6  \w     51.00  77.00   1.00   30.00    --  105.68-125.00 150.00   26
  7  \w     77.00 173.00   1.00   30.00    --  105.68  30.00   0.00   96
  8  \w     43.00 117.00   1.00   30.00    --  105.68-125.00 -30.00   74
  9  \w     34.00 126.00   1.00   30.00    --  105.68 -45.00 -90.00   92
 10  \w     48.00 108.00   1.00   30.00    --  105.68 -94.00  60.00   60
 11  \w     94.00 121.00   1.00   30.00    --  105.68 125.00   0.00   27
 12  \w    146.00 172.00   1.00   30.00    --  105.68 125.00   0.00   26
 13  \w     77.00 177.00   1.00   30.00    --  105.68  30.00 -60.00  100
 14  \w     68.00 108.00   1.00   30.00    --  105.68 -94.00 -30.00   40
 15  \w     29.00 101.00   1.00   30.00    --  105.68 -94.00 150.00   72
 16  \w     29.00 114.00   1.00   30.00    --  105.68 -30.00   0.00   85
 17  \w     41.00 125.00   1.00   30.00    --  105.68 -45.00 120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0295025000
_diffrn_orient_matrix_UB_12      -0.0967847000
_diffrn_orient_matrix_UB_13      -0.0083775000
_diffrn_orient_matrix_UB_21      -0.0313662000
_diffrn_orient_matrix_UB_22      0.0021671000
_diffrn_orient_matrix_UB_23      -0.0351053000
_diffrn_orient_matrix_UB_31      0.0479095000
_diffrn_orient_matrix_UB_32      0.0610161000
_diffrn_orient_matrix_UB_33      -0.0120475000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            45657
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.684
_diffrn_reflns_theta_min         3.696
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.453
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.328
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (Rigaku Oxford Diffraction, 2018).
 Numerical absorption correction based on Gaussian integration over
 a multifaceted crystal model.
 Empirical absorption correction using spherical harmonics
 as implemented in SCALE3 ABSPACK scaling algorithm
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_description       plate
_exptl_crystal_F_000             5160
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.123
_refine_diff_density_min         -1.381
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     776
_refine_ls_number_reflns         12978
_refine_ls_number_restraints     510
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0518
_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^)+(0.0422P)^2^+69.1149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11131
_reflns_number_total             12978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05337_si_003.cif
_cod_data_source_block           ctp463
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        13119.9(4)
_cod_database_code               4128279
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C48 H108 O16 Si4 Tb'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42A-C41 = C42B-C41 = C44B-C41 = C44A-C41 = C43B-C41 = C43A-C41
 1.54 with sigma of 0.02
 C46A-C45 = C46B-C45 = C47A-C45 = C47B-C45 = C48B-C45 = C48A-C45
 1.54 with sigma of 0.02
 Si3-O44A \\sim Si3-O44B
 with sigma of 0.02
 C49-C50A \\sim C50B-C49 \\sim C49-C52A \\sim C52B-C49 \\sim C49-C51A \\sim
C51B-C49
 with sigma of 0.02
 C50A-C51A \\sim C51A-C52A \\sim C52A-C50A \\sim C50B-C51B \\sim C51B-C52B
\\sim C52B-C50B
 with sigma of 0.02
 O44A-C49 \\sim O44B-C49
 with sigma of 0.02
 Si3-O42A \\sim Si3-O42B
 with sigma of 0.02
 Si3-O43A \\sim Si3-O43B
 with sigma of 0.02
 O42A-C41 \\sim O42B-C41
 with sigma of 0.02
 O43A-C45 \\sim O43B-C45
 with sigma of 0.02
 C42A-C44A \\sim C44A-C43A \\sim C43A-C42A \\sim C42B-C44B \\sim C44B-C43B
\\sim C43B-C42B
 with sigma of 0.02
 C46A-C47A \\sim C47A-C48A \\sim C48A-C46A \\sim C46B-C47B \\sim C47B-C48B
\\sim C48B-C46B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O42A \\sim O42B \\sim O43A \\sim O43B \\sim O44A \\sim O44B \\sim C1 \\sim C2
\\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim
C11 \\sim C12 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C41 \\sim C42A
\\sim C42B \\sim C43A \\sim C43B \\sim C44A \\sim C44B \\sim C45 \\sim C46A
\\sim C46B \\sim C47A \\sim C47B \\sim C48A \\sim C48B \\sim C49 \\sim C50A
\\sim C50B \\sim C51A \\sim C51B \\sim C52A \\sim C52B \\sim C61 \\sim C62
\\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70
\\sim C71 \\sim C72: within 2A with sigma of 0.005 and sigma for terminal atoms
of 0.01
4. Others
 Sof(O42B)=Sof(O43B)=Sof(O44B)=Sof(C42B)=Sof(H42D)=Sof(H42E)=Sof(H42F)=
 Sof(C43B)=Sof(H43D)=Sof(H43E)=Sof(H43F)=Sof(C44B)=Sof(H44D)=Sof(H44E)=
 Sof(H44F)=Sof(C46B)=Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47B)=Sof(H47D)=
 Sof(H47E)=Sof(H47F)=Sof(C48B)=Sof(H48D)=Sof(H48E)=Sof(H48F)=Sof(C50B)=
 Sof(H50D)=Sof(H50E)=Sof(H50F)=Sof(C51B)=Sof(H51D)=Sof(H51E)=Sof(H51F)=
 Sof(C52B)=Sof(H52D)=Sof(H52E)=Sof(H52F)=1-FVAR(1)
 Sof(O42A)=Sof(O43A)=Sof(O44A)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(H42C)=
 Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44A)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(H47C)=Sof(C48A)=Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C50A)=
 Sof(H50A)=Sof(H50B)=Sof(H50C)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
 Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
5.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42A(H42A,H42B,H42C),
 C42B(H42D,H42E,H42F), C43A(H43A,H43B,H43C), C43B(H43D,H43E,H43F), C44A(H44A,
 H44B,H44C), C44B(H44D,H44E,H44F), C46A(H46A,H46B,H46C), C46B(H46D,H46E,H46F),
 C47A(H47A,H47B,H47C), C47B(H47D,H47E,H47F), C48A(H48A,H48B,H48C), C48B(H48D,
 H48E,H48F), C50A(H50A,H50B,H50C), C50B(H50D,H50E,H50F), C51A(H51A,H51B,H51C),
 C51B(H51D,H51E,H51F), C52A(H52A,H52B,H52C), C52B(H52D,H52E,H52F), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,H66C),
 C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,H71B,
 H71C), C72(H72A,H72B,H72C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 1.613
_oxdiff_exptl_absorpt_empirical_full_min 0.684