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_1564920
_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         '2(Al C16 F36 O4), C28 H20 As2 Mo4 O8 P2'
_chemical_formula_sum            'C60 H20 Al2 As2 F72 Mo4 O16 P2'
_chemical_formula_weight         3014.26
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-07-27
_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                 90.8706(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.48296(15)
_cell_length_b                   21.4711(2)
_cell_length_c                   26.9785(3)
_cell_measurement_reflns_used    26537
_cell_measurement_temperature    123.1(1)
_cell_measurement_theta_max      73.9100
_cell_measurement_theta_min      3.4980
_cell_volume                     8967.59(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      123.1(1)
_diffrn_detector_area_resol_mean 5.1773
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega -118.00   -9.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0072  -77.0000  -60.0000 109

  2 omega  -30.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0072  -57.0000  150.0000 100

  3 omega   79.00  158.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292   30.0000   90.0000 79

  4 omega   31.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292  -30.0000  -90.0000 38

  5 omega   35.00  136.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292  -61.0000  120.0000 101

  6 omega   31.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292  -30.0000  -30.0000 38

  7 omega   31.00   69.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292  -30.0000  -60.0000 38

  8 omega   24.00  109.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292  -94.0000  120.0000 85

  9 omega   34.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9292 -125.0000  -30.0000 87

 10 omega -115.00  -68.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0072  -57.0000   30.0000 47

 11 omega -115.00  -14.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.0072  -57.0000  150.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0239
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            42829
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.096
_diffrn_reflns_theta_min         3.520
_exptl_absorpt_coefficient_mu    7.820
_exptl_absorpt_correction_T_max  0.602
_exptl_absorpt_correction_T_min  0.349
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
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 dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_exptl_crystal_recrystallization_method 'DCM/alkane layering'
_exptl_crystal_size_max          0.2597
_exptl_crystal_size_mid          0.1438
_exptl_crystal_size_min          0.0999
_refine_diff_density_max         1.851
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1896
_refine_ls_number_reflns         17600
_refine_ls_number_restraints     587
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0682P)^2^+1.8499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0985
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15039
_reflns_number_total             17600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04924k2.cif
_cod_data_source_block           ld106_new_abs_error_model_off
_cod_original_cell_volume        8967.59(15)
_cod_database_code               1564920
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.509
_shelx_estimated_absorpt_t_min   0.236
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F116-C92 = F117-C92 = F115-C92
 1.35 with sigma of 0.02
 F1C-C1A = F1A-C1A = F1B-C1A = F1I-C1C = F1H-C1C = F1G-C1C = F1F-C1B = F1E-C1B
 = F1D-C1B
 1.35 with sigma of 0.02
 C92-C89
 1.53 with sigma of 0.02
 C92-C89 = C91-C89 = C90-C89
 1.53 with sigma of 0.02
 F114-C91 = F113-C91 = F112-C91
 1.35 with sigma of 0.02
 F111-C90 = F110-C90 = F109-C90
 1.35 with sigma of 0.02
 F125-C96 = F124-C96 = F126-C96 = F120-C94 = F119-C94 = F118-C94 = F123-C95 =
 F121-C95 = F122-C95
 1.35 with sigma of 0.02
 C90-C92
 2.55 with sigma of 0.04
 C92-C91
 2.55 with sigma of 0.04
 C91-C90
 2.55 with sigma of 0.04
 O11-C49 \\sim O111-C93
 with sigma of 0.02
 F115-F116 \\sim F116-F117 \\sim F117-F115
 with sigma of 0.02
 F1G-F1H \\sim F1H-F1I \\sim F1I-F1G
 with sigma of 0.02
 F1A-F1B \\sim F1B-F1C \\sim F1C-F1A
 with sigma of 0.02
 F1D-F1E \\sim F1E-F1F \\sim F1F-F1D
 with sigma of 0.02
 C1A-C13 \\sim C1B-C13 \\sim C58-C57 \\sim C1C-C13 \\sim C60-C57 \\sim C59-C57
 with sigma of 0.02
 F64-C70 \\sim F65-C70 \\sim F64-C74 \\sim F75-C74
 with sigma of 0.02
 F70-C72 \\sim F71-C72 \\sim F72-C72 \\sim F81-C76
 with sigma of 0.02
 F68-C71 \\sim F67-C71 \\sim F69-C71 \\sim F76-C75 \\sim F78-C75
 with sigma of 0.02
 C64A-C61A \\sim C64-C61 \\sim C62A-C61A \\sim C62-C61 \\sim C63-C61
 with sigma of 0.02
 C76-C69 \\sim C72-C69 \\sim C75-C69 \\sim C71-C69 \\sim C74-C69 \\sim C70-C69
 with sigma of 0.02
 F47A-C62A \\sim F48A-C62A \\sim F46A-C62A
 with sigma of 0.02
 F54A-C64A \\sim F53A-C64A \\sim F52A-C64A \\sim F52-C64 \\sim F53-C64 \\sim
F54-C64
 with sigma of 0.02
 O14A-C61A \\sim O14-C61
 with sigma of 0.02
 C94-C93 \\sim C96-C93 \\sim C95-C93
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1C \\sim C60 \\sim C57 \\sim C13 \\sim C58 \\sim C1B \\sim C59 \\sim C1A \\sim
O17: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
C1C \\sim F1I \\sim F1H \\sim F1G: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F1F \\sim F1D \\sim F1E \\sim C1B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F1C \\sim C1A \\sim F1A \\sim F1B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C70 \\sim C74 \\sim C69 \\sim C71 \\sim C75 \\sim C72 \\sim C76: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C76 \\sim F81: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
O14A \\sim C61A \\sim C61 \\sim C62 \\sim C62A \\sim C63 \\sim C64A \\sim C64
\\sim O14 \\sim C63A: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C75 \\sim F78 \\sim F76: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C74 \\sim F75: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F52A \\sim F52 \\sim C64A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F49A \\sim C63A \\sim F50A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
F53A \\sim C64A \\sim F52A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
C66 \\sim C78 \\sim C65: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
C80 \\sim C68 \\sim C65 \\sim C66 \\sim C78: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
Al11 \\sim Al1 \\sim O12 \\sim O9: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F46A \\sim F48A \\sim C62A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.7A
4. Others
 Fixed Sof: F37(0.88) F38(0.88) F39(0.88) F40(0.88) F41(0.88) F42(0.88)
 F43(0.88) F44(0.88) F45(0.88) F46(0.86) F47(0.86) F48(0.86) F49(0.86)
 F50(0.86) F52(0.86) F53(0.86) F54(0.86) O13(0.88) O14(0.86) C57(0.88)
 C58(0.88) C59(0.88) C60(0.88) C61(0.86) C62(0.86) C63(0.86) C64(0.86)
 F65(0.81) F67(0.81) F68(0.81) F70(0.81) C70(0.81) C71(0.81) C72(0.81)
 F75(0.19) F76(0.19) F78(0.19) F81(0.19) C74(0.19) C75(0.19) C76(0.19) F56(0.6)
 F57(0.6) F58(0.6) F60(0.6) F62(0.6) F63(0.6) C66(0.6) C68(0.6) F83(0.4)
 F84(0.4) F85(0.4) F87(0.4) F89(0.4) F90(0.4) C78(0.4) C80(0.4) Al1(0.9)
 O10(0.9) F10(0.9) F11(0.9) F12(0.9) F13(0.9) F14(0.9) F15(0.9) F16(0.9)
 F17(0.9) F18(0.9) C45(0.9) C46(0.9) C47(0.9) C48(0.9) F109(0.1) F110(0.1)
 F111(0.1) F112(0.1) F113(0.1) F114(0.1) F115(0.1) F116(0.1) F117(0.1) C89(0.1)
 C90(0.1) C91(0.1) C92(0.1) F19(0.9) F20(0.9) F21(0.9) F22(0.9) F23(0.9)
 F24(0.9) F25(0.9) F26(0.9) F27(0.9) O11(0.9) C49(0.9) C50(0.9) C51(0.9)
 C52(0.9) F118(0.1) F119(0.1) F120(0.1) F121(0.1) F122(0.1) F123(0.1) F124(0.1)
 F125(0.1) F126(0.1) O111(0.1) C93(0.1) C94(0.1) C95(0.1) C96(0.1) O14A(0.14)
 C61A(0.14) C62A(0.14) F47A(0.14) F48A(0.14) F46A(0.14) F52A(0.14) F54A(0.14)
 C64A(0.14) F53A(0.14) C63A(0.14) F49A(0.14) F50A(0.14) O17(0.12) C13(0.12)
 C1A(0.12) F1A(0.12) F1B(0.12) F1C(0.12) C1B(0.12) F1D(0.12) F1E(0.12)
 F1F(0.12) C1C(0.12) F1G(0.12) F1H(0.12) F1I(0.12) O110(0.1) Al11(0.1)
 Fixed Uiso: F109(0.04) F110(0.04) F111(0.04) F112(0.04) F113(0.04) F114(0.04)
 F115(0.04) F116(0.04) F117(0.04) C90(0.04) C91(0.04) C92(0.04) F118(0.03)
 F119(0.03) F120(0.03) F121(0.03) F122(0.03) F123(0.03) F124(0.03) F125(0.03)
 F126(0.03) O111(0.03) C93(0.03) C94(0.03) C95(0.03) C96(0.03)
5.a Aromatic/amide H refined with riding coordinates:
 C0AA(H0AA), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8),
 C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20)
;
_shelx_res_checksum              41062
_shelx_hkl_checksum              45684
_olex2_submission_special_instructions 'No special instructions were received'