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

data_1563605
_publ_section_title
;
 Transfer of Polyantimony Units
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC02498A
_journal_year                    2021
_chemical_formula_moiety         'C26 H42 Sb6 Zr2'
_chemical_formula_sum            'C26 H42 Sb6 Zr2'
_chemical_formula_weight         1267.53
_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             2020-04-15
_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                105.899(7)
_cell_angle_beta                 96.387(6)
_cell_angle_gamma                109.955(8)
_cell_formula_units_Z            1
_cell_length_a                   7.7940(6)
_cell_length_b                   10.9301(11)
_cell_length_c                   11.6145(7)
_cell_measurement_reflns_used    4042
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.3610
_cell_measurement_theta_min      4.5400
_cell_volume                     871.21(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_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     18.00 114.00   1.00    5.00    --   43.98  57.00 150.00   96
  2  \w    -20.00  83.00   1.00    5.00    --   43.98 -99.00 -90.00  103
  3  \w    -26.00  70.00   1.00    5.00    --   43.98 -57.00   0.00   96
  4  \w     31.00 131.00   1.00   20.00    --  104.50 -30.00-180.00  100
  5  \w     31.00 131.00   1.00   20.00    --  104.50 -30.00 -30.00  100
  6  \w     21.00 109.00   1.00   20.00    --  104.50 -94.00-120.00   88
  7  \w     78.00 178.00   1.00   20.00    --  104.50  30.00 150.00  100
  8  \w     21.00 109.00   1.00   20.00    --  104.50 -94.00 150.00   88
  9  \w     31.00 131.00   1.00   20.00    --  104.50 -30.00  90.00  100
 10  \w     30.00 136.00   1.00   20.00    --  104.50 -77.00 -30.00  106
 11  \w     18.00 114.00   1.00    5.00    --   43.98  57.00  60.00   96
 12  \w     18.00 106.00   1.00    5.00    --   43.98  57.00-120.00   88
 13  \w     18.00 114.00   1.00    5.00    --   43.98  57.00 -30.00   96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0528989000
_diffrn_orient_matrix_UB_12      0.0290410000
_diffrn_orient_matrix_UB_13      -0.1186786000
_diffrn_orient_matrix_UB_21      0.0003420000
_diffrn_orient_matrix_UB_22      0.1393978000
_diffrn_orient_matrix_UB_23      0.0771761000
_diffrn_orient_matrix_UB_31      0.2093139000
_diffrn_orient_matrix_UB_32      0.0709333000
_diffrn_orient_matrix_UB_33      0.0029572000
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0466
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6598
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.079
_diffrn_reflns_theta_max         67.079
_diffrn_reflns_theta_min         4.063
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    41.088
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orangish brown'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_description       plate
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.603
_refine_diff_density_rms         0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3080
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0563P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2672
_reflns_number_total             3080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc02498a2.cif
_cod_data_source_block           sean242_brownorange_plate2
_cod_original_cell_volume        871.21(13)
_cod_database_code               1563605
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C26H42Zr2Sb6
_shelx_estimated_absorpt_t_max   0.542
_shelx_estimated_absorpt_t_min   0.233
_reflns_odcompleteness_completeness 99.00
_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:
 C3(H3), C4(H4), C1(H1)
2.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C7(H7a,H7b,H7c), C11(H11a,H11b,H11c), C9(H9a,H9b,H9c),
 C12(H12a,H12b,H12c), C13(H13a,H13b,H13c)
;
_shelx_res_checksum              73391
_shelx_hkl_checksum              43828
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 2.000
_oxdiff_exptl_absorpt_empirical_full_min 0.565