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_1564921
_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 As2.07 Bi1.93 Mo4 O8, 2(Al C16 Cl12 F24 O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C62 H24 Al2 As2.07 Bi1.93 Cl28 F48 Mo4 O16'
_chemical_formula_weight         3925.55
_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             2021-07-28
_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                 96.234(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.3028(2)
_cell_length_b                   27.6708(4)
_cell_length_c                   14.6789(3)
_cell_measurement_reflns_used    25056
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      34.3910
_cell_measurement_theta_min      3.1690
_cell_volume                     5371.34(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.41.21a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.41.21a (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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 7.9851
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.930
_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     39.00 110.00   1.00   15.00    --   32.12 178.00-120.00   71
  2  \w    -15.00  76.00   1.00   15.00    --   32.12 -99.00  60.00   91
  3  \w    -42.00  82.00   1.00   15.00    --   32.12 -19.00  60.00  124
  4  \w     11.00  75.00   1.00   15.00    --   32.12  57.00 120.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            51984
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.590
_diffrn_reflns_theta_min         2.945
_exptl_absorpt_coefficient_mu    5.090
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.106
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.21a (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    2.427
_exptl_crystal_description       block
_exptl_crystal_F_000             3709
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of CH2Cl2 and hexane  by solvent layering'
_exptl_crystal_size_max          0.984
_exptl_crystal_size_mid          0.237
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.920
_refine_diff_density_min         -1.979
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         21333
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0320P)^2^+5.1461P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18316
_reflns_number_total             21333
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc04924k2.cif
_cod_data_source_block           ld448_abs
_cod_database_code               1564921
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.082
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Bi1(0.965) As2(0.035)
3.a Secondary CH2 refined with riding coordinates:
 C201(H20A,H20B)
3.b 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)
;
_shelx_res_checksum              81782
_shelx_hkl_checksum              95195
_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
;