Transfer of Polyantimony Units
Heinl, Veronika; Seitz, Andreas; Balazs, Gabor; Seidl, Michael; Scheer, Manfred; Chemical Science  (2021) –; doi:10.1039/D1SC02498A

data_1563606
_publ_section_title
;
 Transfer of Polyantimony Units
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02498A
_journal_year                    2021
_chemical_formula_moiety         'C51 H87 Fe3 Sb6'
_chemical_formula_sum            'C51 H87 Fe3 Sb6'
_chemical_formula_weight         1598.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-04-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.07.11 svn.r3635 for OlexSys, GUI svn.r5848)
;
_audit_update_record
;
2021-04-23 deposited with the CCDC.	2021-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                93.653(2)
_cell_angle_beta                 101.854(2)
_cell_angle_gamma                104.007(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4528(3)
_cell_length_b                   14.3499(4)
_cell_length_c                   20.1596(5)
_cell_measurement_reflns_used    17186
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      66.4100
_cell_measurement_theta_min      4.1190
_cell_volume                     2850.83(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement
'olex2.refine 1.3-alpha (Bourhis et al., 2015)'
_computing_structure_solution
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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     12.00 115.00   1.00   20.00    --   41.41  57.00 120.00  103
  2  \w     -3.00  96.00   1.00   20.00    --   41.41-125.00 -60.00   99
  3  \w    -34.00  68.00   1.00   20.00    --   41.41 -38.00 -30.00  102
  4  \w      9.00 133.00   1.00   80.00    --   93.50 -92.00 -74.85  124
  5  \w      9.00 133.00   1.00   80.00    --   93.50 -93.00  32.05  124
  6  \w     19.00 124.00   1.00   80.00    --   93.50 -61.00  90.00  105
  7  \w     66.00 168.00   1.00   80.00    --   93.50  45.00  30.00  102
  8  \w     11.00  47.00   1.00   80.00    --   93.50 -95.00 -30.00   36
  9  \w     51.00  80.00   1.00   80.00    --   93.50 -95.00 -30.00   29
 10  \w     97.00 137.00   1.00   80.00    --   93.50  61.00  60.00   40
 11  \w     20.00 113.00   1.00   80.00    --   93.50 -45.00-180.00   93
 12  \w     66.00 132.00   1.00   80.00    --   93.50 -92.00 138.65   66
 13  \w    140.00 166.00   1.00   80.00    --   93.50  61.00  60.00   26
 14  \w     10.00  78.00   1.00   80.00    --   93.50 -95.00-150.00   68
 15  \w     26.00 123.00   1.00   80.00    --   93.50 -61.00  30.00   97
 16  \w     16.00  46.00   1.00   80.00    --   93.50 -30.00  60.00   30
 17  \w     50.00 106.00   1.00   80.00    --   93.50 -30.00  60.00   56
 18  \w     11.00  74.00   1.00   80.00    --   93.50 -95.00-180.00   63
 19  \w     42.00 115.00   1.00   80.00    --   93.50  15.00  30.00   73
 20  \w    125.00 159.00   1.00   80.00    --   93.50  15.00  30.00   34
 21  \w     12.00  59.00   1.00   80.00    --   93.50 -92.00 -16.43   47
 22  \w     65.00 127.00   1.00   80.00    --   93.50 -92.00 -16.43   62
 23  \w     10.00  36.00   1.00   80.00    --   93.50 -92.00 138.65   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0332717000
_diffrn_orient_matrix_UB_12      -0.0818731000
_diffrn_orient_matrix_UB_13      0.0405633000
_diffrn_orient_matrix_UB_21      0.0973367000
_diffrn_orient_matrix_UB_22      0.0756058000
_diffrn_orient_matrix_UB_23      0.0574028000
_diffrn_orient_matrix_UB_31      -0.1172958000
_diffrn_orient_matrix_UB_32      0.0007952000
_diffrn_orient_matrix_UB_33      0.0352828000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29637
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.775
_diffrn_reflns_theta_max         66.775
_diffrn_reflns_theta_min         3.687
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    28.318
_exptl_absorpt_correction_T_max  0.504
_exptl_absorpt_correction_T_min  0.163
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_description       needle
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.169
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.654
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         10011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0223
_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^)+(0.0206P)^2^+0.3101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9103
_reflns_number_total             10011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02498a2.cif
_cod_data_source_block           ap_aps
_cod_database_code               1563606
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C51H87Fe3Sb6
_reflns_odcompleteness_completeness 98.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C4(H4), C35(H35), C1(H1), C18(H18), C38(H38)
2.b Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C25(H25a,H25b,H25c), C15(H15a,H15b,H15c), C30(H30a,H30b,
 H30c), C32(H32a,H32b,H32c), C33(H33a,H33b,H33c), C51(H51a,H51b,H51c), C28(H28a,
 H28b,H28c), C7(H7a,H7b,H7c), C12(H12a,H12b,H12c), C17(H17a,H17b,H17c),
 C11(H11a,H11b,H11c), C29(H29a,H29b,H29c), C45(H45a,H45b,H45c), C50(H50a,H50b,
 H50c), C47(H47a,H47b,H47c), C24(H24a,H24b,H24c), C13(H13a,H13b,H13c), C8(H8a,
 H8b,H8c), C9(H9a,H9b,H9c), C34(H34a,H34b,H34c), C49(H49a,H49b,H49c), C42(H42a,
 H42b,H42c), C16(H16a,H16b,H16c), C43(H43a,H43b,H43c), C41(H41a,H41b,H41c),
 C46(H46a,H46b,H46c)
;
_shelx_res_checksum              74175
_shelx_hkl_checksum              59567
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.847
_oxdiff_exptl_absorpt_empirical_full_min 0.622