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_1564925
_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 As2 Mo4 O8 Sb2, Al C16 F36 O4, Al C14 F31.5 O4, 0.5(C4 F9)'
_chemical_formula_sum            'C60 H20 Al2 As2 F72 Mo4 O16 Sb2'
_chemical_formula_weight         3195.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_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
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.8964(2)
_cell_length_b                   22.20040(10)
_cell_length_c                   29.7016(2)
_cell_measurement_reflns_used    165552
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      37.6710
_cell_measurement_theta_min      1.9140
_cell_volume                     18394.5(2)
_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 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL n/a (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -46.00   3.00   0.50   20.00    --    1.74 -27.00  62.30   98
  2  \w     12.00  44.00   0.50   20.00    --    1.74  58.00 -15.69   64
  3  \w    -23.00  11.00   0.50   20.00    --    1.74 -97.00 135.03   68
  4  \w      9.00  40.00   0.50   20.00    --    1.74  70.00-121.22   62
  5  \w    -11.00  17.00   0.50   20.00    --    1.74 101.00  13.72   56
  6  \w     12.00  44.00   0.50   20.00    --    1.74  57.00  95.66   64
  7  \w    -45.00  -3.00   0.50   20.00    --    2.00 -31.00 -47.28   84
  8  \w    -42.00 -11.00   0.50   20.00    --   -2.36 -66.00  75.85   62
  9  \w     12.00  45.00   0.50   20.00    --    1.74  54.00 -80.94   66
 10  \w    -45.00   6.00   0.50   20.00    --    2.00 -26.00-148.08  102
 11  \w    -45.00 -20.00   0.50   20.00    --    2.00 -31.00  10.58   50
 12  \w     -1.00  45.00   0.50   20.00    --   -2.36  28.00-176.61   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0107812000
_diffrn_orient_matrix_UB_12      0.0178104000
_diffrn_orient_matrix_UB_13      -0.0170447000
_diffrn_orient_matrix_UB_21      0.0084643000
_diffrn_orient_matrix_UB_22      0.0264769000
_diffrn_orient_matrix_UB_23      0.0107386000
_diffrn_orient_matrix_UB_31      0.0214153000
_diffrn_orient_matrix_UB_32      -0.0014946000
_diffrn_orient_matrix_UB_33      -0.0128317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0704
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            437712
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.577
_diffrn_reflns_theta_min         1.835
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.047
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.727
_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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.308
_exptl_crystal_description       block
_exptl_crystal_F_000             12144
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.109
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2548
_refine_ls_number_reflns         33485
_refine_ls_number_restraints     1404
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0345P)^2^+25.1441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0786
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27529
_reflns_number_total             33485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04924k2.cif
_cod_data_source_block           ld461_op_abs_gaus
_cod_database_code               1564925
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C60H20Al2As2F72Mo4O16Sb2
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F52C-C52C = F53C-C52C = F54C-C52C
 1.35 with sigma of 0.02
 F54B-C52B = F53B-C52B = F52B-C52B
 1.35 with sigma of 0.02
 F46B-C50B = F48B-C50B = F47B-C50B
 1.35 with sigma of 0.02
 F44B-C48B = F43B-C48B = F45B-C48B
 1.35 with sigma of 0.02
 F45A-C48A = F43A-C48A = F44A-C48A
 1.35 with sigma of 0.02
 F44C-C48C = F45C-C48C = F43C-C48C
 1.35 with sigma of 0.02
 F41A-C47A \\sim F42A-C47A \\sim F40A-C47A
 with sigma of 0.02
 C44B-C41 \\sim C44A-C41 \\sim C43A-C41 \\sim C43B-C41 \\sim C42-C41
 with sigma of 0.02
 Al2-O16A \\sim Al2-O16B
 with sigma of 0.02
 C59A-C57 \\sim C58A-C57 \\sim C60A-C57
 with sigma of 0.02
 C55B-C53 \\sim C55A-C53 \\sim C56A-C53 \\sim C56B-C53 \\sim C54B-C53 \\sim
C54A-C53
 with sigma of 0.02
 C47A-C45A \\sim C47B-C45B \\sim C47C-C45C \\sim C48A-C45A \\sim C48B-C45B
\\sim C48C-C45C \\sim C46B-
 C45B \\sim C46A-C45A \\sim C46C-C45C
 with sigma of 0.02
 C51B-C49 \\sim C52B-C49 \\sim C50B-C49
 with sigma of 0.02
 Al2-O10 \\sim Al2-O13A
 with sigma of 0.02
 O10-C45C \\sim O13A-C45C
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Mo3A \\sim Mo3B \\sim As2B \\sim As2A \\sim Sb2B \\sim Sb2A \\sim Sb1B \\sim
Sb1A \\sim As1A \\sim As1B \\sim Mo2A \\sim Mo2B: within 3.2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 3.2A
F39C \\sim C47A \\sim F41A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
F44C \\sim F45A \\sim F43C \\sim F45C \\sim C48C: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
F54C \\sim C52C \\sim F52C \\sim F53C: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C44B \\sim F36B \\sim F34B \\sim F35B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F51A \\sim C51A \\sim F49A \\sim F50A \\sim F52C: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
C58B \\sim C58A \\sim C57 \\sim C59A \\sim C59B \\sim C60B \\sim C60A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F19A \\sim C38A \\sim F20A \\sim F21A \\sim C38B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.7A
C43B \\sim F32B \\sim F33B \\sim F31B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C40A \\sim F27A \\sim F27B \\sim C37 \\sim C40B \\sim F25A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
C42 \\sim F28 \\sim F29B \\sim F29A \\sim F30A \\sim F30B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C44A \\sim C44B \\sim C41 \\sim C42 \\sim C43A \\sim C43B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C38B \\sim C38A \\sim C37: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C33A \\sim C33B \\sim C35B \\sim C35A \\sim C36B \\sim C36A \\sim C34A \\sim
C34B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C53 \\sim C55B \\sim C55A \\sim C56A \\sim C56B \\sim C54B \\sim C54A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F61B \\sim C56B \\sim F62B \\sim F63B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F59B \\sim C55B \\sim F60B \\sim F58B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F43A \\sim C48A \\sim F44A \\sim F44B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C48C \\sim C48B \\sim C48A \\sim C45A \\sim C45B \\sim C45C \\sim C47B \\sim
C47A \\sim C47C \\sim C46B \\sim C46A \\sim C46C: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
F64B \\sim C58B \\sim F65B \\sim F66B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C50C \\sim C50B \\sim C49 \\sim C50A \\sim C51C \\sim C51B \\sim C51A \\sim
C52C \\sim C52B \\sim C52A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
F47B \\sim C50B \\sim F48B \\sim F46B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C51C \\sim F49C \\sim F48A \\sim F50C: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F51B \\sim C51B \\sim F49B \\sim F50B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F52A \\sim F54A \\sim C52A \\sim F53A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F46A \\sim C50A \\sim F47A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
C52B \\sim F53B \\sim F54B \\sim F52B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F47C \\sim C50C \\sim F48C \\sim F46C: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
O10 \\sim O13A \\sim Al2: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 2A
F21A \\sim F21B \\sim C38A \\sim C38B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F48A \\sim F51C \\sim C50A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
4. Others
 Fixed Sof: Sb2A(0.8) Sb1A(0.8) Mo1A(0.8) Mo4A(0.8) Mo3A(0.8) Mo2A(0.8)
 As2A(0.8) As1A(0.8) O13A(0.5) F71A(0.7) F62A(0.7) F66A(0.7) F39A(0.5)
 F64A(0.7) O15A(0.7) F45A(0.5) O16A(0.7) F60A(0.7) F72A(0.7) F44A(0.5)
 F65A(0.7) F61A(0.7) F70A(0.7) F69A(0.7) F41A(0.5) F43A(0.5) F63A(0.7)
 F47A(0.47) F67A(0.7) F58A(0.7) F68A(0.7) F51A(0.47) F59A(0.7) F56A(0.7)
 F38A(0.5) F57A(0.7) F48A(0.47) F49A(0.47) F52A(0.47) F54A(0.47) C45A(0.5)
 F37A(0.5) F55A(0.7) F50A(0.47) F42A(0.5) F40A(0.5) C60A(0.7) F46A(0.47)
 C56A(0.7) C58A(0.7) C55A(0.7) F53A(0.47) C59A(0.7) C46A(0.5) C48A(0.5)
 C54A(0.7) C50A(0.47) C51A(0.47) C52A(0.47) O10A(0.5) C33A(0.5) C34A(0.5)
 F11A(0.5) F12A(0.5) F10A(0.5) C36A(0.5) F17A(0.5) F18A(0.5) F16A(0.5)
 C35A(0.5) F15A(0.5) F13A(0.5) F14A(0.5) O10B(0.5) C33B(0.5) C35B(0.5)
 F13B(0.5) F14B(0.5) F15B(0.5) C34B(0.5) F10B(0.5) F11B(0.5) F12B(0.5)
 C36B(0.5) F18B(0.5) F16B(0.5) F17B(0.5) O11A(0.51) C38A(0.51) F20A(0.51)
 F21A(0.51) F19A(0.51) C40A(0.51) F26A(0.51) F27A(0.51) F25A(0.51) C39A(0.51)
 F24A(0.51) F22A(0.51) F23A(0.51) O11B(0.49) C38B(0.49) F20B(0.49) F19B(0.49)
 C40B(0.49) F26B(0.49) F27B(0.49) F25B(0.49) C39B(0.49) F24B(0.49) F22B(0.49)
 F23B(0.49) O12A(0.6) C43A(0.6) F33A(0.6) F31A(0.6) F32A(0.6) F29A(0.6)
 F30A(0.6) C44A(0.6) F36A(0.6) F34A(0.6) F35A(0.6) O12B(0.4) C43B(0.4)
 F33B(0.4) F31B(0.4) F32B(0.4) F29B(0.4) F30B(0.4) C44B(0.4) F36B(0.4)
 F34B(0.4) F35B(0.4) O16B(0.3) C58B(0.3) F66B(0.3) F64B(0.3) F65B(0.3)
 C60B(0.3) F71B(0.3) F72B(0.3) F70B(0.3) C59B(0.3) F67B(0.3) F68B(0.3)
 F69B(0.3) O14A(0.75) C51C(0.29) F49C(0.29) F50C(0.29) C50C(0.29) F47C(0.29)
 F48C(0.29) F46C(0.29) C52C(0.29) F54C(0.29) F52C(0.29) F53C(0.29) O14B(0.25)
 C50B(0.24) F48B(0.24) F46B(0.24) F47B(0.24) C52B(0.24) F53B(0.24) F54B(0.24)
 F52B(0.24) C51B(0.24) F51B(0.24) F49B(0.24) F50B(0.24) O15B(0.3) C55B(0.3)
 F60B(0.3) F58B(0.3) F59B(0.3) C54B(0.3) F56B(0.3) F57B(0.3) F55B(0.3)
 C56B(0.3) F63B(0.3) F61B(0.3) F62B(0.3) C47A(0.5) O13B(0.25) C45B(0.25)
 C47B(0.25) F42B(0.25) F40B(0.25) F41B(0.25) C46B(0.25) F38B(0.25) F39B(0.25)
 F37B(0.25) C48B(0.25) F45B(0.25) F43B(0.25) F44B(0.25) C45C(0.25) C46C(0.25)
 F39C(0.25) F37C(0.25) F38C(0.25) C48C(0.25) F44C(0.25) F45C(0.25) F43C(0.25)
 C47C(0.25) F42C(0.25) F40C(0.25) F41C(0.25) As2B(0.2) Sb2B(0.2) Sb1B(0.2)
 As1B(0.2) Mo2B(0.2) Mo3B(0.2) O10(0.25) F21B(0.49) Mo4B(0.2) Mo1B(0.2)
 F51C(0.29)
5.a Aromatic/amide H refined with riding coordinates:
 C19(H19), C27(H27), C25(H25), C20(H20), C28(H28), C26(H26), C24(H24), C4(H4),
 C5(H5), C18(H18), C6(H6), C7(H7), C17(H17), C3(H3), C21(H21), C11(H11),
 C14(H14), C10(H10), C13(H13), C12(H12)
;
_shelx_res_checksum              84478
_shelx_hkl_checksum              22904
_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 1.728
_oxdiff_exptl_absorpt_empirical_full_min 0.628