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_4128278
_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 K O16 Si4 Tb'
_chemical_formula_sum            'C48 H108 K O16 Si4 Tb'
_chemical_formula_weight         1251.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.2399(10)
_cell_angle_beta                 94.7326(9)
_cell_angle_gamma                91.1183(9)
_cell_formula_units_Z            4
_cell_length_a                   12.94476(13)
_cell_length_b                   20.0897(2)
_cell_length_c                   26.0868(3)
_cell_measurement_reflns_used    38959
_cell_measurement_temperature    100.00(13)
_cell_measurement_theta_max      75.8570
_cell_measurement_theta_min      3.3790
_cell_volume                     6757.78(12)
_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      100.00(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2817
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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   -103.00 -28.00   1.00    2.50    --  -40.85 -38.00 -30.00   75
  2  \w    -84.00  -2.00   1.00    2.50    --  -40.85 125.00-120.00   82
  3  \w    -46.00  33.00   1.00    2.50    --  -40.85  38.00 150.00   79
  4  \w    -61.00  33.00   1.00    2.50    --  -40.85  77.00  60.00   94
  5  \w    -92.00  -2.00   1.00    2.50    --  -40.85 125.00 150.00   90
  6  \w     11.00  38.00   1.00    2.50    --   40.85 -99.00-120.00   27
  7  \w     23.00  50.00   1.00    2.50    --   40.85  38.00  60.00   27
  8  \w     52.00  79.00   1.00    2.50    --   40.85  38.00  60.00   27
  9  \w     66.00 113.00   1.00   10.00    --  112.00-111.00  90.00   47
 10  \w    101.00 156.00   1.00   10.00    --  112.00 111.00 120.00   55
 11  \w     39.00  68.00   1.00   10.00    --  112.00 -94.00-180.00   29
 12  \w     66.00 113.00   1.00   10.00    --  112.00-111.00 -60.00   47
 13  \w     70.00 113.00   1.00   10.00    --  112.00-111.00-150.00   43
 14  \w     87.00 113.00   1.00   10.00    --  112.00-111.00   0.00   26
 15  \w     31.00  57.00   1.00   10.00    --  112.00 -94.00 120.00   26
 16  \w    110.00 178.00   1.00   10.00    --  112.00  30.00 120.00   68
 17  \w     51.00 107.00   1.00   10.00    --  112.00-111.00  60.00   56
 18  \w     39.00 121.00   1.00   10.00    --  112.00 -45.00 150.00   82
 19  \w    118.00 176.00   1.00   10.00    --  112.00 111.00  60.00   58
 20  \w     84.00 110.00   1.00   10.00    --  112.00  61.00 150.00   26
 21  \w    116.00 177.00   1.00   10.00    --  112.00 111.00-150.00   61
 22  \w     68.00 113.00   1.00   10.00    --  112.00-111.00-120.00   45
 23  \w    105.00 135.00   1.00   10.00    --  112.00 -45.00 -60.00   30
 24  \w     38.00  95.00   1.00   10.00    --  112.00 -77.00 120.00   57
 25  \w     84.00 149.00   1.00   10.00    --  112.00  30.00  60.00   65
 26  \w     73.00 112.00   1.00   10.00    --  112.00-111.00 120.00   39
 27  \w    105.00 141.00   1.00   10.00    --  112.00 111.00 -30.00   36
 28  \w     44.00  69.00   1.00   10.00    --  112.00-111.00   0.00   25
 29  \w     77.00 106.00   1.00   10.00    --  112.00 -94.00 -60.00   29
 30  \w     30.00  91.00   1.00   10.00    --  112.00 -94.00   0.00   61
 31  \w     34.00  60.00   1.00   10.00    --  112.00 -94.00 -60.00   26
 32  \w     85.00 178.00   1.00   10.00    --  112.00  30.00 -90.00   93
 33  \w     64.00  90.00   1.00   10.00    --  112.00 -45.00 -60.00   26
 34  \w     70.00  95.00   1.00   10.00    --  112.00 -94.00 120.00   25
 35  \w     66.00 176.00   1.00   10.00    --  112.00  15.00-150.00  110
 36  \w     68.00  93.00   1.00   10.00    --  112.00-111.00 -90.00   25
 37  \w     34.00  77.00   1.00   10.00    --  112.00 -94.00 -30.00   43
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0162143000
_diffrn_orient_matrix_UB_12      0.0642859000
_diffrn_orient_matrix_UB_13      0.0313339000
_diffrn_orient_matrix_UB_21      -0.0602241000
_diffrn_orient_matrix_UB_22      0.0295754000
_diffrn_orient_matrix_UB_23      -0.0472830000
_diffrn_orient_matrix_UB_31      -0.1018687000
_diffrn_orient_matrix_UB_32      -0.0296403000
_diffrn_orient_matrix_UB_33      0.0172000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            73594
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.226
_diffrn_reflns_theta_min         2.749
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.821
_exptl_absorpt_correction_T_max  0.713
_exptl_absorpt_correction_T_min  0.472
_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 colourless'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       prism
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.737
_refine_diff_density_min         -2.974
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1333
_refine_ls_number_reflns         27895
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0850P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1463
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24444
_reflns_number_total             27895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b05337_si_002.cif
_cod_data_source_block           ctp468
_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        6757.77(13)
_cod_database_code               4128278
_shelx_shelxl_version_number     2018/3
_audit_contact_author            'Farzaneh Fadaei Tirani'
_chemical_oxdiff_formula         'C48 H108 K O16 Si4 Tb'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 Si1, O1, Si5, O81
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.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), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), 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), C82(H82A,H82B,H82C), C83(H83A,H83B,
 H83C), C84(H84A,H84B,H84C), C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,
 H88B,H88C), C90(H90A,H90B,H90C), C91(H91A,H91B,H91C), C92(H92A,H92B,H92C),
 C102(H10D,H10E,H10F), C103(H10G,H10H,H10I), C104(H10J,H10K,H10L), C106(H10M,
 H10N,H10O), C107(H10P,H10Q,H10R), C108(H10S,H10T,H10U), C110(H11D,H11E,H11F),
 C111(H11G,H11H,H11I), C112(H11J,H11K,H11L), C122(H12D,H12E,H12F), C123(H12G,
 H12H,H12I), C124(H12J,H12K,H12L), C126(H12M,H12N,H12O), C127(H12P,H12Q,H12R),
 C128(H12S,H12T,H12U), C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,
 H13H,H13I), C142(H14A,H14B,H14C), C143(H14D,H14E,H14F), C144(H14G,H14H,H14I),
 C146(H14J,H14K,H14L), C147(H14M,H14N,H14O), C148(H14P,H14Q,H14R), C150(H15A,
 H15B,H15C), C151(H15D,H15E,H15F), C152(H15G,H15H,H15I)
;
_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 2.605
_oxdiff_exptl_absorpt_empirical_full_min 0.569