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_7129631
_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_formula_moiety         'C39 H45 Mo3 O9 Sb3, C H2 Cl2'
_chemical_formula_sum            'C40 H47 Cl2 Mo3 O9 Sb3'
_chemical_formula_weight         1395.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-29
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2021-11-03 deposited with the CCDC.	2022-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.672(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5370(2)
_cell_length_b                   29.4147(5)
_cell_length_c                   19.2872(3)
_cell_measurement_reflns_used    9040
_cell_measurement_temperature    123.1(1)
_cell_measurement_theta_max      71.4260
_cell_measurement_theta_min      4.6440
_cell_volume                     4759.50(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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_temperature      123.1(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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    -10.00  27.00   1.00   15.00    --   40.03 -19.00-180.00   37
  2  \w    -43.00 -12.00   1.00   15.00    --   40.03 -19.00-180.00   31
  3  \w     -3.00  92.00   1.00   15.00    --   40.03-125.00   0.00   95
  4  \w    -43.00  27.00   1.00   15.00    --   40.03 -19.00-120.00   70
  5  \w     29.00  59.00   1.00   60.00    --  105.16 -61.00-120.00   30
  6  \w     30.00  71.00   1.00   60.00    --  105.16 -61.00-150.00   41
  7  \w     73.00 176.00   1.00   60.00    --  105.16  77.00 120.00  103
  8  \w     39.00  69.00   1.00   60.00    --  105.16 -61.00  30.00   30
  9  \w     87.00 178.00   1.00   60.00    --  105.16  30.00-120.00   91
 10  \w     30.00  70.00   1.00   60.00    --  105.16 -61.00   0.00   40
 11  \w     43.00 104.00   1.00   60.00    --  105.16 -77.00 150.00   61
 12  \w     31.00  83.00   1.00   60.00    --  105.16 -95.00 -30.00   52
;
_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      -0.0939230000
_diffrn_orient_matrix_UB_12      0.0176264000
_diffrn_orient_matrix_UB_13      -0.0708350000
_diffrn_orient_matrix_UB_21      0.1571486000
_diffrn_orient_matrix_UB_22      0.0146568000
_diffrn_orient_matrix_UB_23      -0.0218753000
_diffrn_orient_matrix_UB_31      0.0136717000
_diffrn_orient_matrix_UB_32      -0.0470987000
_diffrn_orient_matrix_UB_33      -0.0333353000
_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  0.0445
_diffrn_reflns_av_unetI/netI     0.0568
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16875
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.804
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    21.023
_exptl_absorpt_correction_T_max  0.738
_exptl_absorpt_correction_T_min  0.593
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.948
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.591
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         8391
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0534P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7322
_reflns_number_total             8391
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06770b2.cif
_cod_data_source_block           heve242_5_abs
_cod_database_code               7129631
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C39Cl2Mo3O9Sb3H45
_shelx_estimated_absorpt_t_max   0.262
_shelx_estimated_absorpt_t_min   0.157
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18A-C19A \\sim C18B-C19B
 with sigma of 0.02
 C18A-C23A \\sim C18B-C23B
 with sigma of 0.02
 C21A-C20A \\sim C21B-C20B
 with sigma of 0.02
 C21A-C26A \\sim C21B-C26B
 with sigma of 0.02
 C19A-C20A \\sim C19B-C20B
 with sigma of 0.02
 C19A-C24A \\sim C19B-C24B
 with sigma of 0.02
 C20A-C25A \\sim C20B-C25B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C17 \\sim C18A \\sim C21A \\sim C19A \\sim C22A \\sim C20A \\sim C26A \\sim
C25A \\sim C24A \\sim C25B \\sim C20B \\sim C21B \\sim C26B \\sim C19B \\sim
C18B \\sim C23B \\sim C24B \\sim C23A \\sim C22B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
4. Others
 Fixed Sof: C18A(0.5) C21A(0.5) C19A(0.5) C22A(0.5) H22A(0.5) H22B(0.5)
 H22C(0.5) C20A(0.5) C26A(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C25A(0.5)
 H25A(0.5) H25B(0.5) H25C(0.5) C23A(0.5) H23A(0.5) H23B(0.5) H23C(0.5)
 C24A(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C25B(0.5) H25D(0.5) H25E(0.5)
 H25F(0.5) C20B(0.5) C21B(0.5) C26B(0.5) H26D(0.5) H26E(0.5) H26F(0.5)
 C22B(0.5) H22D(0.5) H22E(0.5) H22F(0.5) C19B(0.5) C18B(0.5) C23B(0.5)
 H23D(0.5) H23E(0.5) H23F(0.5) C24B(0.5) H24D(0.5) H24E(0.5) H24F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B)
5.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C37(H37A,H37B,H37C), C36(H36A,H36B,
 H36C), C9(H9A,H9B,H9C), C39(H39A,H39B,H39C), C35(H35A,H35B,H35C), C10(H10A,
 H10B,H10C), C13(H13A,H13B,H13C), C38(H38A,H38B,H38C), C22A(H22A,H22B,H22C),
 C26A(H26A,H26B,H26C), C25A(H25A,H25B,H25C), C23A(H23A,H23B,H23C), C24A(H24A,
 H24B,H24C), C25B(H25D,H25E,H25F), C26B(H26D,H26E,H26F), C22B(H22D,H22E,H22F),
 C23B(H23D,H23E,H23F), C24B(H24D,H24E,H24F)
;
_shelx_res_checksum              42865
_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 1.550
_oxdiff_exptl_absorpt_empirical_full_min 0.582