Synthesis of polyantimony ligand complexes starting from Cp*4Sb4
Heinl, Veronika; Balázs, Gábor; Seidl, Michael; Scheer, Manfred; Chemical Communications  (2022) –; doi:10.1039/D1CC06770B

data_7129632
_publ_section_title
;
 Synthesis of polyantimony ligand complexes starting from Cp*4Sb4
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06770B
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C76 H116 Fe4 O8 Sb4'
_chemical_formula_sum            'C76 H116 Fe4 O8 Sb4'
_chemical_formula_weight         1868.08
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-19
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6383)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   27.8565(5)
_cell_length_b                   13.9634(3)
_cell_length_c                   20.9861(4)
_cell_measurement_reflns_used    18782
_cell_measurement_temperature    132(13)
_cell_measurement_theta_max      66.8760
_cell_measurement_theta_min      4.4900
_cell_volume                     8163.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      132(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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     25.00  55.00   1.00   10.00    --   43.41 -92.00 178.00   30
  2  \w    109.00 152.00   1.00   30.00    --   86.50  32.00 113.00   43
  3  \w   -104.00 -53.00   1.00   30.00    --  -90.00  92.00 -69.00   51
  4  \w   -147.00-108.00   1.00   30.00    --  -90.00-159.00 -55.00   39
  5  \w     28.00  69.00   1.00   10.00    --   43.41 -57.00  60.00   41
  6  \w     29.00  98.00   1.00   10.00    --   43.41  57.00 -90.00   69
  7  \w   -157.00-119.00   1.00   30.00    --  -90.00-125.00   0.00   38
  8  \w   -130.00 -97.00   1.00   30.00    --  -90.00-125.00  90.00   33
  9  \w   -163.00-136.00   1.00   30.00    --  -90.00-125.00 150.00   27
 10  \w    -62.00 -35.00   1.00   30.00    --  -90.00  51.00 174.57   27
 11  \w    -79.00 -52.00   1.00   30.00    --  -90.00  30.00-180.00   27
 12  \w   -158.00-115.00   1.00   30.00    --  -90.00 -68.00 -65.33   43
 13  \w   -160.00-105.00   1.00   30.00    --  -90.00-125.00 120.00   55
 14  \w    -94.00 -62.00   1.00   30.00    --  -90.00 112.00-167.57   32
 15  \w   -128.00 -23.00   1.00   30.00    --  -90.00  15.00-120.00  105
 16  \w   -114.00 -64.00   1.00   30.00    --  -90.00 -66.00-132.83   50
 17  \w   -116.00 -91.00   1.00   30.00    --  -90.00  30.00-180.00   25
 18  \w   -159.00-125.00   1.00   30.00    --  -90.00 -59.00 -83.19   34
 19  \w   -163.00-138.00   1.00   30.00    --  -90.00-125.00  90.00   25
 20  \w   -149.00-122.00   1.00   30.00    --  -90.00 -94.00 120.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0191196000
_diffrn_orient_matrix_UB_12      0.0393014000
_diffrn_orient_matrix_UB_13      -0.0850809000
_diffrn_orient_matrix_UB_21      -0.0126128000
_diffrn_orient_matrix_UB_22      0.0549716000
_diffrn_orient_matrix_UB_23      0.0686146000
_diffrn_orient_matrix_UB_31      0.0503538000
_diffrn_orient_matrix_UB_32      0.0286565000
_diffrn_orient_matrix_UB_33      -0.0148894000
_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  0.0791
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45225
_diffrn_reflns_point_group_measured_fraction_full 0.835
_diffrn_reflns_point_group_measured_fraction_max 0.835
_diffrn_reflns_theta_full        66.875
_diffrn_reflns_theta_max         66.875
_diffrn_reflns_theta_min         3.802
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.236
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.277
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
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            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.520
_exptl_crystal_description       block
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.118
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.073
_refine_diff_density_max         1.626
_refine_diff_density_min         -1.504
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.050(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         12117
_refine_ls_number_restraints     306
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0633
_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^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1425
_reflns_Friedel_coverage         0.633
_reflns_Friedel_fraction_full    0.668
_reflns_Friedel_fraction_max     0.668
_reflns_number_gt                10566
_reflns_number_total             12117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06770b2.cif
_cod_data_source_block           heve389_op_abs
_cod_database_code               7129632
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         '(C19 H29 Fe Sb O2)4'
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.950(12)
 0.050(12)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
3. Restrained distances
 C8A-C3 \\sim C8B-C3
 with sigma of 0.02
 C15A-C12 \\sim C15B-C12
 with sigma of 0.02
 C16B-C17B \\sim C17A-C16A \\sim C16B-C18B \\sim C18A-C16A \\sim C19-C16A
 with sigma of 0.02
 C16A-C6 \\sim C16B-C6
 with sigma of 0.02
 Fe1-C1A \\sim Fe1-C1B \\sim Fe1-C2B \\sim Fe1-C2A
 with sigma of 0.02
 C9A-C8A \\sim C11A-C8A \\sim C8B-C9B \\sim C11B-C8B \\sim C10A-C8A \\sim
C10B-C8B
 with sigma of 0.02
 O2B-C2A \\sim O2A-C2B \\sim O1A-C1A \\sim O1B-C1B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C14 \\sim C12 \\sim C13 \\sim C15B \\sim C15A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
C16B \\sim C18B \\sim C18A \\sim C16A \\sim C17A \\sim C17B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
O2B \\sim C2A \\sim C2B \\sim O2A \\sim O1A \\sim O1B \\sim C1B \\sim C1A \\sim
Fe1: within 2.2A with sigma of 0.01 and sigma for terminal atoms of 0.01 within
2.2A
C9B \\sim C9A \\sim C8A \\sim C8B \\sim C10A \\sim C10B \\sim C7 \\sim C11A
\\sim C11B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 1.7A
5. Others
 Fixed Sof: O1A(0.42) O2B(0.58) C16A(0.55) H19A(0.55) H19B(0.55) H19C(0.55)
 H19D(0.45) H19E(0.45) H19F(0.45) C8A(0.63) C18A(0.55) H18A(0.55) H18B(0.55)
 H18C(0.55) C2A(0.42) C17A(0.55) H17A(0.55) H17B(0.55) H17C(0.55) C10A(0.63)
 H10A(0.63) H10B(0.63) H10C(0.63) C1A(0.42) C11A(0.63) H11A(0.63) H11B(0.63)
 H11C(0.63) C9A(0.63) H9AA(0.63) H9AB(0.63) H9AC(0.63) C1B(0.58) O1B(0.58)
 C2B(0.58) O2A(0.42) C9B(0.37) H9BA(0.37) H9BB(0.37) H9BC(0.37) C8B(0.37)
 C10B(0.37) H10D(0.37) H10E(0.37) H10F(0.37) C11B(0.37) H11D(0.37) H11E(0.37)
 H11F(0.37) C15A(0.58) H15A(0.58) H15B(0.58) H15C(0.58) C15B(0.42) H15D(0.42)
 H15E(0.42) H15F(0.42) C16B(0.45) C17B(0.45) H17D(0.45) H17E(0.45) H17F(0.45)
 C18B(0.45) H18D(0.45) H18E(0.45) H18F(0.45)
6.a Aromatic/amide H refined with riding coordinates:
 C62(H62), C26(H26), C43(H43), C45(H45), C7(H7), C5(H5), C64(H64), C24(H24)
6.b Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C70(H70A,H70B,H70C), C49(H49A,H49B,H49C), C67(H67A,H67B,
 H67C), C51(H51A,H51B,H51C), C71(H71A,H71B,H71C), C57(H57A,H57B,H57C), C53(H53A,
 H53B,H53C), C68(H68A,H68B,H68C), C48(H48A,H48B,H48C), C72(H72A,H72B,H72C),
 C19(H19A,H19B,H19C), C19(H19D,H19E,H19F), C37(H37A,H37B,H37C), C52(H52A,H52B,
 H52C), C18A(H18A,H18B,H18C), C55(H55A,H55B,H55C), C76(H76A,H76B,H76C),
 C74(H74A,H74B,H74C), C47(H47A,H47B,H47C), C14(H14A,H14B,H14C), C29(H29A,H29B,
 H29C), C17A(H17A,H17B,H17C), C10A(H10A,H10B,H10C), C56(H56A,H56B,H56C),
 C30(H30A,H30B,H30C), C75(H75A,H75B,H75C), C32(H32A,H32B,H32C), C13(H13A,H13B,
 H13C), C66(H66A,H66B,H66C), C34(H34A,H34B,H34C), C11A(H11A,H11B,H11C),
 C28(H28A,H28B,H28C), C38(H38A,H38B,H38C), C36(H36A,H36B,H36C), C9A(H9AA,H9AB,
 H9AC), C9B(H9BA,H9BB,H9BC), C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F),
 C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C17B(H17D,H17E,H17F), C18B(H18D,
 H18E,H18F)
;
_shelx_res_checksum              6964
_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 3.575
_oxdiff_exptl_absorpt_empirical_full_min 0.453