Structural Diversity of Mixed Polypnictogen Complexes: Dicationic E2E'2 (E, E' = P, As, Sb, Bi) Chains, Cycles and Cages Stabilized by Transition Metals
Dütsch, Luis; Riesinger, Christoph; Balazs, Gabor; Seidl, Michael; Scheer, Manfred; Chemical Science  (2021) –; doi:10.1039/D1SC04924K

data_1564924
_publ_section_title
;
 Structural Diversity of Mixed Polypnictogen Complexes: Dicationic E2E'2
 (E, E' = P, As, Sb, Bi) Chains, Cycles and Cages Stabilized by Transition
 Metals
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC04924K
_journal_year                    2021
_chemical_formula_moiety         'C28 H20 Bi2 Mo4 O8 Sb2, 2(Al C16 F36 O4)'
_chemical_formula_sum            'C60 H20 Al2 Bi2 F72 Mo4 O16 Sb2'
_chemical_formula_weight         3463.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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
;
2021-08-24 deposited with the CCDC.	2021-10-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.5124(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.58714(13)
_cell_length_b                   22.64745(18)
_cell_length_c                   25.9896(2)
_cell_measurement_reflns_used    51577
_cell_measurement_temperature    110.00(12)
_cell_measurement_theta_max      74.1330
_cell_measurement_theta_min      2.2740
_cell_volume                     9174.20(13)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_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     -5.00  34.00   1.00   10.00    --  -43.39  19.00-180.00   39
  2  \w     -5.00  34.00   1.00   10.00    --  -43.39  19.00 -30.00   39
  3  \w    -22.00  28.00   1.00   10.00    --  -43.39  38.00  30.00   50
  4  \w     61.00 133.00   1.00   10.00    --   43.39 178.00-120.00   72
  5  \w    103.00 178.00   1.00   40.00    --  104.50  77.00-150.00   75
  6  \w     34.00  72.00   1.00   40.00    --  104.50 -45.00-180.00   38
  7  \w     31.00  57.00   1.00   40.00    --  104.50 -30.00  60.00   26
  8  \w     35.00  93.00   1.00   40.00    --  104.50 -61.00 -30.00   58
  9  \w    103.00 178.00   1.00   40.00    --  104.50  77.00 -90.00   75
 10  \w     31.00 112.00   1.00   40.00    --  104.50-125.00  90.00   81
 11  \w     78.00 174.00   1.00   40.00    --  104.50  61.00   0.00   96
 12  \w     34.00  72.00   1.00   40.00    --  104.50 -45.00 -90.00   38
 13  \w     35.00  93.00   1.00   40.00    --  104.50 -61.00-120.00   58
 14  \w     31.00  57.00   1.00   40.00    --  104.50 -30.00 150.00   26
 15  \w   -113.00 -18.00   1.00   10.00    --  -43.39 -57.00-120.00   95
 16  \w   -113.00 -18.00   1.00   10.00    --  -43.39 -57.00 150.00   95
 17  \w   -113.00 -18.00   1.00   10.00    --  -43.39 -57.00  30.00   95
 18  \w     65.00 109.00   1.00   40.00    --  104.50  15.00 150.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0525189000
_diffrn_orient_matrix_UB_12      0.0443128000
_diffrn_orient_matrix_UB_13      -0.0199151000
_diffrn_orient_matrix_UB_21      0.0696412000
_diffrn_orient_matrix_UB_22      0.0236787000
_diffrn_orient_matrix_UB_23      -0.0260704000
_diffrn_orient_matrix_UB_31      -0.0192636000
_diffrn_orient_matrix_UB_32      -0.0354121000
_diffrn_orient_matrix_UB_33      -0.0423515000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0457
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            84463
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         74.128
_diffrn_reflns_theta_min         2.337
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.899
_exptl_absorpt_correction_T_max  0.642
_exptl_absorpt_correction_T_min  0.079
_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            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_description       block
_exptl_crystal_F_000             6472
_exptl_crystal_size_max          0.373
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.086
_refine_diff_density_max         2.412
_refine_diff_density_min         -1.794
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1694
_refine_ls_number_reflns         24730
_refine_ls_number_restraints     656
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0592P)^2^+83.6952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1532
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23965
_reflns_number_total             24730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04924k2.cif
_cod_data_source_block           ld364_mp_abs_gaus
_cod_database_code               1564924
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C60H20Al2Bi2F72Mo4O16Sb2
_shelx_estimated_absorpt_t_max   0.381
_shelx_estimated_absorpt_t_min   0.078
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C65-C35 \\sim C66-C65 \\sim C65-C30 \\sim C67-C65 \\sim C68-C65 \\sim C65-C29
 with sigma of 0.02
 F64-C70 \\sim F164-C70 \\sim F65-C70 \\sim F165-C70 \\sim F66-C70 \\sim
F166-C70
 with sigma of 0.02
 Bi1-Sb1 \\sim Bi1A-Sb1A
 with sigma of 0.02
 C69-C172 \\sim C72-C69 \\sim C69-C171 \\sim C71-C69 \\sim C70-C69
 with sigma of 0.02
 F68-C71 \\sim F67-C71 \\sim F69-C71
 with sigma of 0.02
 F168-C171 \\sim F167-C171 \\sim F69-C171
 with sigma of 0.02
 F170-C172 \\sim F172-C172 \\sim F171-C172 \\sim F72-C72 \\sim F70-C72 \\sim
F71-C72
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C18 \\sim C18A \\sim C19 \\sim C19A \\sim C15 \\sim C15A \\sim C16 \\sim C16A
\\sim C17A \\sim C17: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C70 \\sim F64 \\sim F164 \\sim F65 \\sim F165 \\sim F166 \\sim F66: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
Sb2A \\sim Bi2 \\sim Sb2 \\sim Bi2A \\sim Bi1 \\sim Sb1A \\sim Sb1 \\sim Bi1A:
within 3.4A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.4A
C171 \\sim C71 \\sim C69 \\sim C72 \\sim C172 \\sim C70: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F167 \\sim C171 \\sim F168: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C66 \\sim C35 \\sim C65 \\sim C67 \\sim C30 \\sim C68 \\sim C29: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F58 \\sim F77 \\sim C67 \\sim C30 \\sim F59 \\sim F76: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F78 \\sim C35 \\sim F79 \\sim F80: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C172 \\sim F171 \\sim F172 \\sim F170: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F72 \\sim C72 \\sim F70 \\sim F71: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F67 \\sim F68 \\sim C71 \\sim F69: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
4. Others
 Sof(Bi2A)=Sof(Sb2A)=Sof(Sb1A)=Sof(Bi1A)=1-FVAR(1)
 Sof(Bi1)=Sof(Bi2)=Sof(Sb1)=Sof(Sb2)=FVAR(1)
 Fixed Sof: C15(0.59) H15(0.59) C16(0.59) H16(0.59) C17(0.59) H17(0.59)
 C18(0.59) H18(0.59) C19(0.59) H19(0.59) F64(0.48) F65(0.48) F66(0.48)
 F67(0.48) F68(0.48) F70(0.48) F71(0.48) F72(0.48) C71(0.48) C72(0.48)
 F164(0.52) F165(0.52) F166(0.52) F167(0.52) F168(0.52) F170(0.52) F171(0.52)
 F172(0.52) C171(0.52) C172(0.52) F55(0.72) F56(0.72) F57(0.72) F58(0.72)
 F59(0.72) F61(0.72) F62(0.72) F63(0.72) C66(0.72) C67(0.72) C68(0.72)
 F73(0.28) F74(0.28) F75(0.28) F76(0.28) F77(0.28) F78(0.28) F79(0.28)
 F80(0.28) C29(0.28) C30(0.28) C35(0.28) C15A(0.41) H15A(0.41) C17A(0.41)
 H17A(0.41) C18A(0.41) H18A(0.41) C19A(0.41) H19A(0.41) C16A(0.41) H16A(0.41)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26), C15A(H15A), C17A(H17A), C18A(H18A), C19A(H19A),
 C16A(H16A)
;
_shelx_res_checksum              40841
_shelx_hkl_checksum              89925
_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 2.316
_oxdiff_exptl_absorpt_empirical_full_min 0.626