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_1564923
_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
'C14 H10 As Bi Mo2 O4, C14 H9 As1.12 Bi0.88 Mo2 O4, 2(Al C16 F36 O4), 0.1(C H2 Cl2)'
_chemical_formula_sum
'C60.1 H19.2 Al2 As2.12 Bi1.88 Cl0.2 F72 Mo4 O16'
_chemical_formula_weight         3361.68
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                80.965(3)
_cell_angle_beta                 82.393(2)
_cell_angle_gamma                75.244(2)
_cell_formula_units_Z            2
_cell_length_a                   14.9100(3)
_cell_length_b                   15.9359(6)
_cell_length_c                   20.4158(7)
_cell_measurement_reflns_used    13072
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      33.5290
_cell_measurement_theta_min      3.6350
_cell_volume                     4611.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.27a (Rigaku OD, 2019)'
_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
'olex2.solve 1.3-alpha (Bourhis et al., 2015)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_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   -114.00  65.00   1.00   12.50    --  -24.77   0.00 150.00  179
  2  \w     30.00  86.00   1.00   12.50    --   26.49-128.00 -47.00   56
  3  \w     -7.00  39.00   1.00   12.50    --   26.49  77.00  30.00   46
  4  \w     61.00 117.00   1.00   12.50    --   26.49 178.00 -90.00   56
  5  \w     38.00  94.00   1.00   12.50    --   26.49-142.00 141.00   56
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            48635
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.366
_exptl_absorpt_coefficient_mu    5.088
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.354
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.27a (Rigaku Oxford Diffraction, 2019)
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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    2.421
_exptl_crystal_description       rod
_exptl_crystal_F_000             3158
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of CH2Cl2 and hexane  by solvent layering'
_exptl_crystal_size_max          0.606
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.387
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2440
_refine_ls_number_reflns         27938
_refine_ls_number_restraints     1724
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0437
_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^)+(0.0322P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0920
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20441
_reflns_number_total             27938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04924k2.cif
_cod_data_source_block           cr500_moa
_cod_original_formula_sum
'C60.10 H19.20 Al2 As2.12 Bi1.88 Cl0.20 F72 Mo4 O16'
_cod_database_code               1564923
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.558
_shelx_estimated_absorpt_t_min   0.149
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl3-C61 = Cl2-C61
 1.75 with sigma of 0.02
 F55A-C54A = F56A-C54A = F57A-C54A
 1.35 with sigma of 0.01
 F24B-C39B \\sim F24A-C39A \\sim F23B-C39B \\sim F23A-C39A \\sim F22B-C39B
\\sim C39A-F22A
 with sigma of 0.02
 C42A-C41 \\sim C44B-C41 \\sim C44A-C41 \\sim C43B-C41 \\sim C43A-C41 \\sim
C42B-C41
 with sigma of 0.02
 F30B-C42B \\sim F28B-C42B \\sim F29B-C42B \\sim F30A-C42A \\sim F28A-C42A
\\sim F29A-C42A
 with sigma of 0.02
 F22A-F24A \\sim F24A-F23A \\sim F23A-F22A
 with sigma of 0.02
 F29B-F28B \\sim F28B-F30B \\sim F30B-F29B
 with sigma of 0.02
 F38A-C46 \\sim F38B-C46 \\sim F39A-C46 \\sim F39B-C46 \\sim F37-C46
 with sigma of 0.02
 C36B-C33 \\sim C36A-C33 \\sim C33-C36C \\sim C35B-C33 \\sim C35A-C33 \\sim
C33-C35C \\sim C34B-C33 ~
 C34A-C33 \\sim C33-C34C
 with sigma of 0.02
 F57A-F56A \\sim F56A-F55A \\sim F55A-F57A
 with sigma of 0.02
 F17C-C36C \\sim F16C-C36C \\sim F18C-C36C \\sim F16A-C36A \\sim F17A-C36A
\\sim F17B-C36B \\sim F18A-
 C36A \\sim F18B-C36B \\sim F16B-C36B
 with sigma of 0.02
 F15B-C35B \\sim F13B-C35B \\sim F13A-C35A \\sim F14A-C35A \\sim F14B-C35B
\\sim F15A-C35A \\sim F13C-
 C35C \\sim F15C-C35C \\sim F14C-C35C
 with sigma of 0.02
 F33B-C43B \\sim F31-C43B \\sim F32B-C43B
 with sigma of 0.02
 F11C-C34C \\sim F10C-C34C \\sim F10A-C34A \\sim F11B-C34B \\sim F11A-C34A
\\sim F12C-C34C \\sim F12A-
 C34A \\sim F12B-C34B \\sim F10B-C34B
 with sigma of 0.02
 F6B-C31B \\sim F5B-C31B \\sim F4B-C31B \\sim F2B-C30B \\sim F1B-C30B \\sim
F3B-C30B \\sim F7B-C32B ~
 F8B-C32B \\sim F9B-C32B
 with sigma of 0.02
 C31B-C29 \\sim C30B-C29 \\sim C32B-C29
 with sigma of 0.02
 F25B-C40B \\sim F25A-C40A \\sim F27-C40B \\sim F26B-C40B \\sim F26A-C40A
 with sigma of 0.02
 C38A-C37 \\sim C38B-C37 \\sim C39A-C37 \\sim C39B-C37 \\sim C40A-C37 \\sim
C40B-C37
 with sigma of 0.02
 C38A-F21A \\sim C38A-F19A \\sim C38A-F20A
 with sigma of 0.02
 C38A-C40A \\sim C40A-C39A \\sim C39A-C38A
 with sigma of 0.02
 F21A-F19A \\sim F19A-F20A \\sim F20A-F21A
 with sigma of 0.02
 O13B-C45 \\sim O13A-C45
 with sigma of 0.02
 C57-C59B \\sim C59A-C57 \\sim C60A-C57 \\sim C57-C60B \\sim C58A-C57 \\sim
C57-C58B
 with sigma of 0.02
 F68B-C59B \\sim F69B-C59B \\sim F67B-C59B
 with sigma of 0.02
 F72B-C60B \\sim F70B-C60B \\sim F71B-C60B
 with sigma of 0.02
 F64B-C58B \\sim F65B-C58B \\sim F66B-C58B \\sim F65A-C58A \\sim F66A-C58A
\\sim F64A-C58A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F24B \\sim F23B \\sim F23A \\sim C39B \\sim C39A \\sim F22B \\sim F22A \\sim
F24A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.7A
C43B \\sim F32A \\sim F33B \\sim F32B \\sim C43A \\sim F33A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
C41 \\sim C43A \\sim C43B \\sim C42B \\sim C42A \\sim C44B \\sim C44A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
C42B \\sim F28B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F56A \\sim C54A \\sim F57A \\sim F55A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F30A \\sim F30B \\sim C42B \\sim C42A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F55A \\sim F56B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
O10 \\sim O10A \\sim C33 \\sim C34A \\sim C34B \\sim C34C \\sim C36B \\sim C36A
\\sim C36C \\sim C35B \\sim C35A \\sim C35C: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
F39B \\sim F39A \\sim C46 \\sim F38B \\sim F38A: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.01 within 1.7A
As3 \\sim Bi2 \\sim As3 \\sim Bi2 \\sim As2: within 2.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2.7A
F14C \\sim C35C \\sim F13C \\sim F15C \\sim F15B \\sim C35B \\sim F13B \\sim
F14B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.7A
F11C \\sim F11B \\sim C34C \\sim C34B \\sim F10B \\sim F10C \\sim F12C \\sim
F12B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.7A
F17C \\sim F17B \\sim C36C \\sim F18C \\sim F16C \\sim F16B \\sim C36B \\sim
F18B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.7A
F27 \\sim C40B \\sim C40A \\sim F26A \\sim F25A \\sim F25B \\sim F26B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C29 \\sim C32B \\sim C32A \\sim C31B \\sim C31A \\sim C30B \\sim C30A \\sim
O9A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
1.7A
F6B \\sim C31B \\sim F5B \\sim F4B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F2B \\sim C30B \\sim F1B \\sim F3B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C25A \\sim C24 \\sim C24A \\sim C23A \\sim C23 \\sim C22 \\sim C22A \\sim C26
\\sim C26A \\sim C25: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
F8B \\sim C32B \\sim F7B \\sim F9B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F21B \\sim F21A \\sim C38B \\sim F19A \\sim F19B \\sim C38A \\sim F20B \\sim
F20A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
C56B \\sim C53A \\sim C56A \\sim C53B \\sim C54A \\sim C54B \\sim C55B \\sim
C55A \\sim O15: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
C40B \\sim C40A \\sim C38B \\sim C38A \\sim C37 \\sim C39A \\sim C39B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C61 \\sim Cl3 \\sim Cl2: within 1.9A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.9A
F59A \\sim C55A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
F61B \\sim F60A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F58A \\sim F63B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F57B \\sim C54B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C48B \\sim C48A \\sim C45 \\sim C47A \\sim C47B \\sim C46: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C58B \\sim C58A \\sim C57 \\sim C59B \\sim C59A \\sim C60B \\sim C60A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F71B \\sim C60B \\sim F72B \\sim F70B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F64B \\sim C58B \\sim F66B \\sim F65B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F69B \\sim C59B \\sim F67B \\sim F68B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
4. Others
 Fixed Sof: Bi2(0.88) F7A(0.86) F9A(0.86) F8A(0.86) F5A(0.86) F4A(0.86)
 F6A(0.86) F3A(0.86) F2A(0.86) F1A(0.86) F36A(0.74) F33A(0.74) F32A(0.74)
 F29A(0.74) F28A(0.74) F21A(0.12) F19A(0.12) F20A(0.12) F26A(0.12) F25A(0.12)
 F22A(0.12) F24A(0.12) F23A(0.12) F10A(0.55) F12A(0.55) F11A(0.55) F16A(0.55)
 F18A(0.55) F17A(0.55) F14A(0.55) F13A(0.55) F15A(0.55) O9(0.86) O10A(0.88)
 C22(0.52) HN(0.52) C23(0.52) HO(0.52) C24(0.52) HP(0.52) C25(0.52) HQ(0.52)
 C26(0.52) HR(0.52) C32A(0.86) C31A(0.86) C30A(0.86) C44A(0.74) C43A(0.74)
 C42A(0.74) C38A(0.12) C40A(0.12) C39A(0.12) C34A(0.55) C36A(0.55) C35A(0.55)
 F44A(0.5) F45A(0.5) F43A(0.5) F39B(0.5) F38B(0.5) F40A(0.5) F41A(0.5)
 F42A(0.5) F51A(0.578) F52A(0.578) F53A(0.578) F46A(0.578) F47A(0.578)
 F48A(0.578) F60A(0.5) F59A(0.5) F58A(0.5) F62A(0.5) F63A(0.5) F61A(0.5)
 F57A(0.5) F56A(0.5) F55A(0.5) F67A(0.629) F68A(0.629) F69A(0.629) F71A(0.629)
 F72A(0.629) F70A(0.629) F64A(0.629) F65A(0.629) F66A(0.629) O13A(0.5)
 O16A(0.629) C48A(0.5) C47A(0.5) C51A(0.578) C52A(0.578) C50A(0.578) C53A(0.5)
 C55A(0.5) C56A(0.5) C54A(0.5) C59A(0.629) C60A(0.629) C58A(0.629) F45B(0.5)
 F43B(0.5) F44B(0.5) F39A(0.5) F38A(0.5) F40B(0.5) F41B(0.5) F42B(0.5)
 F51B(0.422) F52B(0.422) F53B(0.422) F54B(0.422) F47B(0.422) F46B(0.422)
 F62B(0.5) F61B(0.5) F63B(0.5) F55B(0.5) F56B(0.5) F57B(0.5) F60B(0.5)
 F58B(0.5) F59B(0.5) F68B(0.371) F69B(0.371) F67B(0.371) F70B(0.371)
 F71B(0.371) F72B(0.371) F65B(0.371) F66B(0.371) F64B(0.371) O13B(0.5)
 O16B(0.371) C48B(0.5) C47B(0.5) C51B(0.422) C52B(0.422) C50B(0.422) C53B(0.5)
 C56B(0.5) C54B(0.5) C55B(0.5) C59B(0.371) C60B(0.371) C58B(0.371) As3(0.12)
 C22A(0.48) HS(0.48) C26A(0.48) HT(0.48) C25A(0.48) HU(0.48) C24A(0.48)
 HV(0.48) C23A(0.48) HW(0.48) Cl2(0.1) Cl3(0.1) C61(0.1) HX(0.1) HY(0.1)
 C42B(0.26) F30A(0.74) F29B(0.26) F28B(0.26) C43B(0.26) F32B(0.26) F33B(0.26)
 C44B(0.26) F36B(0.26) F16B(0.31) C36B(0.31) F18B(0.31) F17B(0.31) F13B(0.31)
 C35B(0.31) F15B(0.31) F14B(0.31) F10B(0.31) F12B(0.31) C34B(0.31) F11B(0.31)
 O10(0.12) C35C(0.14) F14C(0.14) F13C(0.14) F15C(0.14) C36C(0.14) F18C(0.14)
 F17C(0.14) F16C(0.14) C34C(0.14) F11C(0.14) F10C(0.14) F12C(0.14) F9B(0.14)
 C32B(0.14) F8B(0.14) F7B(0.14) F6B(0.14) C31B(0.14) F4B(0.14) F5B(0.14)
 F3B(0.14) C30B(0.14) F2B(0.14) F1B(0.14) O9A(0.14) F21B(0.88) F19B(0.88)
 F20B(0.88) F26B(0.88) F25B(0.88) F22B(0.88) F24B(0.88) F23B(0.88) C38B(0.88)
 C40B(0.88) C39B(0.88) F30B(0.26)
5.a Secondary CH2 refined with riding coordinates:
 C61(HX,HY)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H), C2(HA), C3(HB), C4(HC), C5(HD), C8(HE), C9(HF), C10(HG), C11(HH),
 C12(HI), C15(HJ), C16(HK), C17(HL), C19(HM), C22(HN), C23(HO), C24(HP),
 C25(HQ), C26(HR), C22A(HS), C26A(HT), C25A(HU), C24A(HV), C23A(HW)
;
_shelx_res_checksum              8800
_shelx_hkl_checksum              47035
_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
;