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_1564922
_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, 2(Al C16 Cl12 F24 O4)'
_chemical_formula_sum            'C60 H20 Al2 As2 Cl24 F48 Mo4 O16 Sb2'
_chemical_formula_weight         3590.62
_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
_audit_creation_date             2021-07-28
_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                 112.9690(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6398(2)
_cell_length_b                   23.2138(2)
_cell_length_c                   23.1270(2)
_cell_measurement_reflns_used    33990
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      73.8630
_cell_measurement_theta_min      3.8590
_cell_volume                     10202.27(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_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      123.00(10)
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.967
_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    -24.00  69.00   1.00    2.50    --   44.92 -57.00-120.00   93
  2  \w    -27.00  75.00   1.00    2.50    --   44.92 -77.00  30.00  102
  3  \w     73.00 176.00   1.00   10.00    --  104.50 125.00   0.00  103
  4  \w     23.00 109.00   1.00   10.00    --  104.50 -94.00   0.00   86
  5  \w     68.00 178.00   1.00   10.00    --  104.50  15.00  60.00  110
  6  \w     33.00 121.00   1.00   10.00    --  104.50-125.00-150.00   88
  7  \w     82.00 173.00   1.00   10.00    --  104.50  45.00 120.00   91
  8  \w     15.00 117.00   1.00    2.50    --   44.92  77.00-150.00  102
  9  \w     21.00 113.00   1.00    2.50    --   44.92  57.00 -30.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58041
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.031
_diffrn_reflns_theta_min         3.808
_exptl_absorpt_coefficient_mu    16.089
_exptl_absorpt_correction_T_max  0.719
_exptl_absorpt_correction_T_min  0.477
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41h (Rigaku Oxford Diffraction, 2015)
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    2.338
_exptl_crystal_description       block
_exptl_crystal_F_000             6840
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of CH2Cl2 and hexane  by solvent layering'
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1675
_refine_ls_number_reflns         20043
_refine_ls_number_restraints     587
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0769P)^2^+22.0108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1233
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18107
_reflns_number_total             20043
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04924k2.cif
_cod_data_source_block           ld196_cr014_abs
_cod_original_cell_volume        10202.27(17)
_cod_database_code               1564922
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.271
_shelx_estimated_absorpt_t_min   0.096
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F6A-C31A \\sim F4A-C31A \\sim F5A-C31A \\sim F4B-C31B \\sim F5B-C31B \\sim
F3A-C30A \\sim F1A-C30A ~
 F2A-C30A \\sim F2B-C30B \\sim F3B-C30B \\sim F1B-C30B
 with sigma of 0.02
 Al2-O14A \\sim Al2-O14
 with sigma of 0.02
 C30B-C29 \\sim C30A-C29 \\sim C31A-C29 \\sim C31B-C29 \\sim C32B-C29 \\sim
C32A-C29
 with sigma of 0.02
 Al1-O12B \\sim Al1-O12A
 with sigma of 0.02
 Cl2-C32A \\sim Cl3A-C32A \\sim Cl1-C32A \\sim Cl3B-C32B
 with sigma of 0.02
 C44B-F23B \\sim C44B-F24B \\sim C44B-F22B
 with sigma of 0.02
 F23B-F24B \\sim F24B-F22B \\sim F22B-F23B
 with sigma of 0.03
 C42A-C41A \\sim C42B-C41B \\sim C44A-C41A \\sim C43-C41A
 with sigma of 0.02
 C44B-C41B \\sim C42B-C41B \\sim C44A-C41A \\sim C43-C41A \\sim C42A-C41A
 with sigma of 0.02
 Sb2-As2 \\sim Sb2B-As2B \\sim Sb1-As1 \\sim Sb1B-As1B
 with sigma of 0.02
 Sb2B-As1B \\sim Sb1-As2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F25 \\sim C46 \\sim F26 \\sim F27: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
F36 \\sim C52: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
C53 \\sim O15A \\sim O15 \\sim Al2: within 1.8A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.8A
C30B \\sim C29 \\sim C30A \\sim C31B \\sim C31A \\sim C32B \\sim C32A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
F22B \\sim C44B \\sim F23B \\sim F24B \\sim C41B: within 1.99A with sigma of
0.01 and sigma for terminal atoms of 0.01 within 1.99A
F3B \\sim F1B \\sim C30B \\sim F2B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F20B \\sim C43: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.7A
F19B \\sim F21B \\sim C43: within 1.99A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.99A
C44B \\sim C41B \\sim C41A \\sim C43 \\sim C44A \\sim C42B: within 1.99A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.99A
C42B \\sim Cl10 \\sim Cl1A: within 1.99A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.99A
Sb1B \\sim As1 \\sim As1B \\sim Sb1 \\sim Sb2B \\sim As2 \\sim As2B \\sim Sb2:
within 3.2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.2A
C11 \\sim C12 \\sim C10 \\sim C9 \\sim C8: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 1.7A
Cl1B \\sim Cl21 \\sim C54: within 1.99A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.99A
Al1: within 3A with sigma of 0.0001 and sigma for terminal atoms of 0.0002
within 3A
Uanis(O14A) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.02
Uanis(F4B) \\sim Ueq, Uanis(F5B) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.005
Uanis(F20B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.003
Uanis(F3B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(F22B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.005
Uanis(C25) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.003 and sigma for terminal
atoms of 0.01
Uanis(C41A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(O12A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
Uanis(O12B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Cl21(0.7) O14(0.6) Cl11(0.85) Cl12(0.85) F20A(0.85) F21A(0.85)
 F19A(0.85) F22A(0.85) F23A(0.85) F24A(0.85) C41A(0.85) C42A(0.85) C44A(0.85)
 Cl3A(0.85) F1A(0.85) F2A(0.85) F4A(0.85) F5A(0.85) C30A(0.85) O15A(0.5)
 O15(0.5) Cl3(0.15) C42B(0.15) Cl1A(0.15) C41B(0.15) F19B(0.15) F21B(0.15)
 F20B(0.15) Sb2(0.84) Sb1(0.84) As2(0.84) As1(0.84) C32A(0.85) C31A(0.85)
 F6A(0.85) As2B(0.16) Sb2B(0.16) Sb1B(0.16) As1B(0.16) C44B(0.15) F23B(0.15)
 F24B(0.15) F22B(0.15) C32B(0.15) Cl3B(0.15) C31B(0.15) F4B(0.15) F5B(0.15)
 C30B(0.15) F2B(0.15) F3B(0.15) F1B(0.15) O12A(0.45) O12B(0.55) Cl1B(0.3)
 O14A(0.4)
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)
;
_shelx_res_checksum              84363
_shelx_hkl_checksum              63990
_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
- Detector area scaling
;