Novel synthetic route towards heteroleptic pnictogen-rich organometallic-inorganic coordination compounds
Shelyganov, Pavel; El Sayed Moussa, Mehdi; Seidl, Michael; Zimmermann, Lisa; Silva, Wagner; Scheer, Manfred; Dalton Transactions  (2023) –; doi:10.1039/D3DT03490A

data_7714527
_publ_section_title
;
 Novel synthetic route towards heteroleptic pnictogen-rich
 organometallic-inorganic coordination compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03490A
_journal_year                    2023
_chemical_formula_moiety
'C56 H40 Ag2 Mo8 O16 P4 Sb4, 2(Al C16 F36 O4), 3(C H2 Cl2)'
_chemical_formula_sum            'C91 H46 Ag2 Al2 Cl6 F72 Mo8 O24 P4 Sb4'
_chemical_formula_weight         4752.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-09-04
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.3940(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.54110(10)
_cell_length_b                   29.9273(4)
_cell_length_c                   21.4675(3)
_cell_measurement_reflns_used    24403
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      32.1330
_cell_measurement_theta_min      2.0890
_cell_volume                     6766.37(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.76a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.76a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5096
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -97.00   9.00   0.50   10.00    --  -19.91 -38.00  30.00  212
  2  \w    -22.00  58.00   0.50   10.00    --  -19.91  38.00-180.00  160
  3  \w    -13.00  39.00   0.50   10.00    --   21.62  77.00  60.00  104
  4  \w   -110.00 -67.00   0.50   10.00    --  -19.91 178.00 -60.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, AtlasS2, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0574650000
_diffrn_orient_matrix_UB_12      0.0020961000
_diffrn_orient_matrix_UB_13      0.0157876000
_diffrn_orient_matrix_UB_21      0.0350241000
_diffrn_orient_matrix_UB_22      0.0018725000
_diffrn_orient_matrix_UB_23      0.0288106000
_diffrn_orient_matrix_UB_31      0.0023582000
_diffrn_orient_matrix_UB_32      0.0235416000
_diffrn_orient_matrix_UB_33      -0.0037203000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            46336
_diffrn_reflns_point_group_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.017
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.120
_exptl_absorpt_correction_T_max  0.764
_exptl_absorpt_correction_T_min  0.396
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.76a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.332
_exptl_crystal_description       plate
_exptl_crystal_F_000             4508
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.46
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.266
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2657
_refine_ls_number_reflns         31124
_refine_ls_number_restraints     1839
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0563P)^2^+10.8146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.824
_reflns_Friedel_fraction_full    0.912
_reflns_Friedel_fraction_max     0.854
_reflns_number_gt                28398
_reflns_number_total             31124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03490a2.cif
_cod_data_source_block           psh166_mo_mp_nc_abs_ana
_cod_database_code               7714527
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Ag2Al2C91Cl6F72Mo8O24P4Sb4
_shelx_estimated_absorpt_t_max   0.756
_shelx_estimated_absorpt_t_min   0.373
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.62(2)
 0.38(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C12A-C14A = C13A-C11A
 2.35 with sigma of 0.02
 C6B-C3B
 2.35 with sigma of 0.02
 C12A-C10A
 2.35 with sigma of 0.02
 C7B-C4B
 2.35 with sigma of 0.02
 F35B-C67B \\sim F36B-C67B \\sim F36A-C67A \\sim F34B-C67B \\sim F34A-C67A
\\sim F35A-C67A
 with sigma of 0.02
 F31-F33B \\sim F33B-F32 \\sim F32-F31
 with sigma of 0.02
 F45B-C71B \\sim F43B-C71B \\sim F44B-C71B \\sim F41B-C70B \\sim F42B-C70B
\\sim F40B-C70B \\sim F39B-
 C69B \\sim F37B-C69B \\sim F38B-C69B
 with sigma of 0.04
 Cl6A-C86A \\sim Cl6B-C86B \\sim Cl5B-C86B \\sim Cl5A-C86A
 with sigma of 0.02
 F34B-F35B \\sim F35B-F36B \\sim F36B-F34B
 with sigma of 0.02
 F45B-F43B \\sim F43B-F44B \\sim F44B-F45B
 with sigma of 0.02
 F29A-C65A \\sim F30-C65A \\sim F28A-C65A \\sim F29B-C65B \\sim F28B-C65B \\sim
F30-C65B
 with sigma of 0.02
 F26A-C63A \\sim F25A-C63A \\sim F27A-C63A \\sim F25B-C63B \\sim F26B-C63B
\\sim F27B-C63B
 with sigma of 0.02
 F47A-C73 \\sim F48A-C73 \\sim F46-C73
 with sigma of 0.02
 C21A-C20A \\sim C21B-C20B \\sim C21A-C17A \\sim C17B-C21B \\sim C17B-C18B
\\sim C18A-C17A \\sim C18A-
 C19A \\sim C19B-C18B \\sim C20A-C19A \\sim C19B-C20B
 with sigma of 0.02
 F25B-F26B \\sim F26B-F27B \\sim F27B-F25B
 with sigma of 0.02
 F43A-C71A \\sim F44A-C71A \\sim F45A-C71A \\sim F41A-C70A \\sim F42A-C70A
\\sim F40A-C70A \\sim F39A-
 C69A \\sim F37A-C69A \\sim F38A-C69A
 with sigma of 0.04
 F43A-F44A \\sim F44A-F45A \\sim F45A-F43A
 with sigma of 0.02
 C68-C71B \\sim C68-C70B \\sim C68-C69B
 with sigma of 0.04
 C70B-C68 \\sim C70A-C68 \\sim C71B-C68 \\sim C71A-C68 \\sim C68-C69A \\sim
C69B-C68
 with sigma of 0.04
 C17B-C21B \\sim C17B-C18B \\sim C19B-C18B \\sim C19B-C20B \\sim C21B-C20B
 with sigma of 0.02
 C3B-C4B \\sim C4B-C5B \\sim C7B-C6B \\sim C5B-C6B \\sim C3B-C7B \\sim C3A-C4A
 with sigma of 0.02
 C14A-C10A \\sim C13A-C14A \\sim C12A-C13A \\sim C12A-C11A \\sim C11A-C10A
 with sigma of 0.02
 O2B-C2B \\sim O2A-C2A
 with sigma of 0.02
 Mo2A-C8A \\sim Mo2B-C8B
 with sigma of 0.02
 Mo1B-C2B \\sim Mo1A-C2A
 with sigma of 0.02
 C4B-C6B \\sim C5B-C7B
 with sigma of 0.02
 C3A-C4A \\sim C4A-C5A \\sim C6A-C5A \\sim C7A-C6A \\sim C7A-C3A
 with sigma of 0.02
 Cl4A-C85A \\sim Cl3B-C85B \\sim Cl3A-C85A \\sim Cl4B-C85B
 with sigma of 0.02
 O3A-C8A \\sim O3B-C8B
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
F35A \\sim C67A \\sim F35B \\sim F36A \\sim F36B \\sim F34B \\sim F34A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
Mo1B \\sim Mo1A \\sim Mo2A \\sim Mo2B: within 3.3A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 3.3A
F33B \\sim C66B \\sim F32: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
Cl6A \\sim C86A \\sim Cl5A \\sim Cl6B \\sim C86B \\sim Cl5B: within 1.9A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.9A
F44A \\sim F45A \\sim C71A \\sim F44B \\sim F43A \\sim C71B \\sim F43B \\sim
F45B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
F25B \\sim C63B \\sim F26B \\sim F27B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C64 \\sim C65B \\sim C65A \\sim C66B \\sim C66A \\sim C67A \\sim C67B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F29A \\sim C65A \\sim F30 \\sim F28A \\sim F29B \\sim F28B \\sim C65B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
O20A \\sim O20B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C70A \\sim C71A \\sim C69A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
F48B \\sim F48A \\sim F46 \\sim C73 \\sim F47A \\sim F47B: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C19A \\sim C19B \\sim C20A \\sim C20B \\sim C21A \\sim C21B \\sim C17B \\sim
C17A \\sim C18B \\sim C18A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
C68 \\sim C69B \\sim C69A \\sim C71B \\sim C71A \\sim C70B \\sim C70A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C13A \\sim C14A \\sim C10A \\sim C17 \\sim C11A \\sim C7 \\sim C12A \\sim C20
\\sim C61 \\sim C62: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.7A
F41A \\sim C70A \\sim F41B \\sim F42A \\sim F42B \\sim F40B \\sim F40A \\sim
C70B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
F38A \\sim F37B \\sim C69A \\sim F37A \\sim C69B \\sim F38B \\sim F39A \\sim
F39B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
O3B \\sim O3A \\sim C8B \\sim C8A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.02 within 1.7A
C2B \\sim C2A \\sim O2A \\sim O2B: within 1.9A with sigma of 0.02 and sigma for
terminal atoms of 0.02 within 1.9A
C7B \\sim C3B \\sim C4B \\sim C5B \\sim C1A \\sim C6B \\sim O1A: within 1.9A
with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
C56 \\sim C59 \\sim C57 \\sim C58: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
C85B \\sim Cl4B \\sim Cl3B \\sim C85A \\sim Cl4A \\sim Cl3A: within 1.9A with
sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.9A
F15B \\sim F15A \\sim C58 \\sim F13A \\sim F13B \\sim F14B \\sim F14A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F18 \\sim F16A \\sim F16B \\sim F17A \\sim F17B \\sim C59: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F10A \\sim F10B \\sim F11B \\sim C57 \\sim F11A \\sim F12B \\sim F12A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
C60 \\sim C62B \\sim C62A \\sim C63A \\sim C63B \\sim C61B \\sim C61A: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
C62B \\sim F22B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F20B \\sim C61B \\sim F21B \\sim F19B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F5A \\sim C54A \\sim F6A \\sim F4 \\sim F5B \\sim C54B \\sim F6B: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
F8A \\sim C55A \\sim F8B \\sim F9A \\sim F7 \\sim C55B \\sim F9B: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
F2A \\sim C53A \\sim F3A \\sim F1 \\sim F2B \\sim C53B \\sim F3B: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
O19B \\sim O19A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
Uanis(C2B) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.08
5. Others
 Fixed Sof: Mo3A(0.52) Mo2A(0.76) Mo1A(0.76) Cl4A(0.75) Cl6A(0.8) Cl5A(0.8)
 Cl3A(0.75) F48A(0.68) O3A(0.76) O2A(0.76) C8A(0.76) C2A(0.76) C17(0.76)
 H17(0.76) F47A(0.68) C61(0.76) H61(0.76) C20(0.76) H20(0.76) C1A(0.76)
 C85A(0.75) H85A(0.75) H85B(0.75) C19A(0.52) H19A(0.52) C20A(0.52) H20A(0.52)
 C62(0.76) H62(0.76) C5A(0.76) H5A(0.76) C7(0.76) H7(0.76) C4A(0.76) H4A(0.76)
 C17A(0.52) H17A(0.52) C6A(0.76) H6A(0.76) C18A(0.52) H18A(0.52) C3A(0.76)
 H3A(0.76) O1A(0.76) C7A(0.76) H7A(0.76) C21A(0.52) H21A(0.52) C86A(0.8)
 H86A(0.8) H86B(0.8) Mo1B(0.24) Mo2B(0.24) C71A(0.55) F43A(0.55) F44A(0.55)
 F45A(0.55) C70A(0.55) F41A(0.55) F42A(0.55) F40A(0.55) C69A(0.55) F39A(0.55)
 F37A(0.55) F38A(0.55) C53A(0.5) F2A(0.5) F3A(0.5) C55A(0.5) F8A(0.5) F9A(0.5)
 C54A(0.5) F5A(0.5) F6A(0.5) C53B(0.5) F2B(0.5) F3B(0.5) C55B(0.5) F9B(0.5)
 F8B(0.5) C54B(0.5) F5B(0.5) F6B(0.5) C18B(0.48) H18B(0.48) C17B(0.48)
 H17B(0.48) C21B(0.48) H21B(0.48) C20B(0.48) H20B(0.48) C19B(0.48) H19B(0.48)
 Mo3B(0.48) F12A(0.46) F10A(0.46) F11A(0.46) F16B(0.54) F17B(0.54) F14A(0.46)
 F15A(0.46) F13A(0.46) F10B(0.54) F12B(0.54) F11B(0.54) F16A(0.46) F17A(0.46)
 F15B(0.54) F14B(0.54) F13B(0.54) O20A(0.71) C67A(0.71) F34A(0.71) F35A(0.71)
 F36A(0.71) C66A(0.71) F33A(0.71) C65A(0.71) F29A(0.71) F28A(0.71) O20B(0.29)
 C67B(0.29) F34B(0.29) F35B(0.29) F36B(0.29) C66B(0.29) F33B(0.29) C65B(0.29)
 F29B(0.29) F28B(0.29) C12A(0.24) H12A(0.24) C13A(0.24) H13A(0.24) C14A(0.24)
 H14A(0.24) C10A(0.24) H10A(0.24) C11A(0.24) H11A(0.24) C8B(0.24) O3B(0.24)
 O19A(0.7) C62A(0.7) F22A(0.7) C61A(0.7) F19A(0.7) F20A(0.7) F21A(0.7)
 C63A(0.7) F25A(0.7) F26A(0.7) F27A(0.7) O19B(0.3) C62B(0.3) F22B(0.3)
 C61B(0.3) F19B(0.3) F20B(0.3) F21B(0.3) C63B(0.3) F25B(0.3) F26B(0.3)
 F27B(0.3) C3B(0.24) H3B(0.24) C7B(0.24) H7B(0.24) C6B(0.24) H6B(0.24)
 C5B(0.24) H5B(0.24) C4B(0.24) H4B(0.24) C2B(0.24) O2B(0.24) C1B(0.24)
 O1B(0.24) C71B(0.45) F45B(0.45) F43B(0.45) F44B(0.45) C70B(0.45) F41B(0.45)
 F42B(0.45) F40B(0.45) C69B(0.45) F39B(0.45) F37B(0.45) F38B(0.45) F48B(0.32)
 F47B(0.32) Cl6B(0.2) Cl5B(0.2) C86B(0.2) H86C(0.2) H86D(0.2) Cl4B(0.25)
 Cl3B(0.25) C85B(0.25) H85C(0.25) H85D(0.25)
6.a Ternary CH refined with riding coordinates:
 C18A(H18A), C21A(H21A), C20B(H20B)
6.b Secondary CH2 refined with riding coordinates:
 C85A(H85A,H85B), C84(H84A,H84B), C86A(H86A,H86B), C86B(H86C,H86D), C85B(H85C,
 H85D)
6.c Aromatic/amide H refined with riding coordinates:
 C53(H53), C46(H46), C45(H45), C55(H55), C1(H1), C42(H42), C49(H49), C5(H5),
 C24(H24), C17(H17), C54(H54), C61(H61), C38(H38), C47(H47), C35(H35), C32(H32),
  C25(H25), C26(H26), C40(H40), C20(H20), C34(H34), C41(H41), C48(H48),
 C27(H27), C28(H28), C19A(H19A), C39(H39), C20A(H20A), C33(H33), C62(H62),
 C31(H31), C5A(H5A), C7(H7), C4A(H4A), C17A(H17A), C6A(H6A), C3A(H3A), C7A(H7A),
  C18B(H18B), C17B(H17B), C21B(H21B), C19B(H19B), C12A(H12A), C13A(H13A),
 C14A(H14A), C10A(H10A), C11A(H11A), C3B(H3B), C7B(H7B), C6B(H6B), C5B(H5B),
 C4B(H4B)
;
_shelx_res_checksum              95081
_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 1.229
_oxdiff_exptl_absorpt_empirical_full_min 0.866