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_7714530
_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 As1.71 Mo8 O16 P6.29, 2(Al C16 F36 O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C90 H44 Ag2 Al2 As1.71 Cl4 F72 Mo8 O24 P6.29'
_chemical_formula_weight         4379.18
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.12.21 svn.raa29eb21 for OlexSys, GUI svn.r6440)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.1327(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.29414(7)
_cell_length_b                   59.0562(5)
_cell_length_c                   21.43082(15)
_cell_measurement_reflns_used    91564
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.5370
_cell_measurement_theta_min      2.5730
_cell_volume                     13025.95(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.118a (Rigaku OD, 2021)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.889
_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     -3.00  55.00   0.25    8.00    --    6.97  41.00-126.00  232
  2  \w    -40.00  12.00   0.25    8.00    --    6.97 -41.00  80.00  208
  3  \w      9.00  40.00   0.25    8.00    --   -7.59  41.00-126.00  124
  4  \w    -65.00  -3.00   0.25    8.00    --   -7.59 -41.00  80.00  248
  5  \w    -21.00  41.00   0.25    8.00    --    6.97 -99.00 -90.00  248
  6  \w    -20.00  41.00   0.25    8.00    --    6.97 -99.00   0.00  244
  7  \w    -26.00  42.00   0.25    8.00    --   -7.59  77.00 -90.00  272
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0576058000
_diffrn_orient_matrix_UB_12      -0.0056422000
_diffrn_orient_matrix_UB_13      0.0088361000
_diffrn_orient_matrix_UB_21      -0.0285715000
_diffrn_orient_matrix_UB_22      0.0024175000
_diffrn_orient_matrix_UB_23      -0.0296423000
_diffrn_orient_matrix_UB_31      0.0247833000
_diffrn_orient_matrix_UB_32      -0.0103261000
_diffrn_orient_matrix_UB_33      -0.0117853000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.889
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       71
_diffrn_reflns_limit_k_min       -85
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            189366
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.889
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.696
_diffrn_reflns_theta_min         2.233
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.118a (Rigaku Oxford Diffraction, 2021)
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 orange'
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_description       block
_exptl_crystal_F_000             8395
_exptl_crystal_size_max          0.147
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.795
_refine_diff_density_min         -0.918
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2764
_refine_ls_number_reflns         42599
_refine_ls_number_restraints     849
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0313P)^2^+39.9258P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0977
_reflns_Friedel_coverage         0.000
_reflns_number_gt                33996
_reflns_number_total             42599
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03490a2.cif
_cod_data_source_block           psh404_mo_mp_abs
_cod_original_cell_volume        13025.94(16)
_cod_database_code               7714530
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C90H44Ag2Al2As1.7Cl4F72Mo8O24P6.3
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.777
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 F7B-C60B = F8B-C60B = F9B-C60B
 1.35 with sigma of 0.01
 Cl6-Cl5
 2.916 with sigma of 0.03
 Cl5-C92
 1.77 with sigma of 0.02
 Cl6-C92 = Cl5-C92
 1.771 with sigma of 0.01
 Cl6-C92
 1.78 with sigma of 0.02
 Cl6-Cl5
 2.92 with sigma of 0.04
 F30A-C70A \\sim F28A-C70A \\sim F29A-C70A \\sim F35A-C72A \\sim F36A-C72A
\\sim F34A-C72A \\sim F33A-
 C71A \\sim F31A-C71A \\sim F32A-C71A
 with sigma of 0.02
 F33C-C71C \\sim F31C-C71C \\sim F32C-C71C \\sim F28C-C70C \\sim F29C-C70C
\\sim F30C-C70C \\sim F36C-
 C72C \\sim F34C-C72C \\sim F35C-C72C
 with sigma of 0.02
 F30B-C70B \\sim F28B-C70B \\sim F29B-C70B \\sim F34B-C72B \\sim F35B-C72B
\\sim F36B-C72B \\sim F32B-
 C71B \\sim F33B-C71B \\sim F31B-C71B
 with sigma of 0.02
 C69C-C71C \\sim C69C-C70C \\sim C69C-C72C
 with sigma of 0.02
 C57B-F7B \\sim C57B-F9B \\sim C57B-F8B
 with sigma of 0.01
 F7B-F9B \\sim F9B-F8B \\sim F8B-F7B
 with sigma of 0.02
 C69B-C70B \\sim C69B-C72B \\sim C69B-C71B
 with sigma of 0.02
 F30B-F28B \\sim F28B-F29B \\sim F29B-F30B
 with sigma of 0.02
 C71B-C69B \\sim C70B-C69B \\sim C72A-C69A \\sim C71A-C69A \\sim C70A-C69A
 with sigma of 0.02
 C69A-C70A \\sim C69A-C72A \\sim C69A-C71A
 with sigma of 0.02
 C89A-C86 \\sim C89B-C86 \\sim C88A-C86 \\sim C88B-C86
 with sigma of 0.02
 F69A-C88A \\sim F69B-C88B \\sim F67-C88B \\sim F67-C88A \\sim F68B-C88B \\sim
F68A-C88A
 with sigma of 0.02
 F70B-C89A \\sim F72B-C89A \\sim F71B-C89A \\sim F3-C89B \\sim F2-C89B \\sim
F1-C89B
 with sigma of 0.02
 C58A-C57A \\sim C57B-C58B \\sim C60A-C57A \\sim C57B-C60B \\sim C59A-C57A
\\sim C57B-C59B
 with sigma of 0.02
 C63B-C61B \\sim C63A-C61A \\sim C62A-C61A \\sim C62B-C61B \\sim C61A-C64
 with sigma of 0.02
 O17-C57B \\sim O17-C57A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
F8B \\sim F9A \\sim C60A \\sim C60B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F34A \\sim C72A \\sim F36A \\sim F35A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F4B \\sim C59B \\sim F5B \\sim F6: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
F5A \\sim C59A \\sim F4A \\sim F6: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
F30B \\sim C70B \\sim F28B \\sim F29B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F9B \\sim C60B \\sim F8B \\sim F7B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C69B \\sim C69A \\sim C71A \\sim C70A \\sim C70B \\sim C72A \\sim C71B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F36B \\sim C72B \\sim F34B \\sim F35B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F32A \\sim C71A \\sim F33A \\sim F31A \\sim F32B \\sim C71B \\sim F33B \\sim
F31B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.7A
O20B \\sim O20A \\sim O1: within 2.2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2.2A
C69A \\sim C69B \\sim C69C: within 2.2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2.2A
As7 \\sim P7 \\sim As8 \\sim P8: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 2.5A
C88A \\sim C88B \\sim C86 \\sim C87A \\sim C87B \\sim C89A \\sim C89B: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.7A
F64B \\sim F64A \\sim C87A \\sim C87B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F69B \\sim F69A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C60A \\sim C60B \\sim C57A \\sim C57B \\sim C59B \\sim C59A \\sim C58A \\sim
C58B: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.7A
Cl6 \\sim Cl5 \\sim C92: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
Al2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
F53B \\sim F52A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F50B \\sim F48A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F51B \\sim F50A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
F60B \\sim F60A: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C84A \\sim C84B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
C62B \\sim C62A \\sim C61B \\sim C61A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
P5 \\sim As5 \\sim As6 \\sim P6: within 2.5A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2.5A
Uanis(As8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Rigid body (RIGU) restrains
 Cl6, Cl5, C92
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: As7(0.63) As6(0.53) P5(0.66) P8(0.79) Cl4(0.5) Cl3(0.5) F17A(0.75)
 F16A(0.75) F48A(0.5) F52A(0.5) F18A(0.75) F1A(0.75) F3A(0.75) F47A(0.5)
 F50A(0.5) F2A(0.75) F51A(0.5) F7A(0.75) F72B(0.5) F46A(0.5) F8A(0.75)
 F53A(0.5) F49A(0.5) C57A(0.75) F70B(0.5) O1A(0.57) C58A(0.75) C6A(0.57)
 F71B(0.5) C60A(0.75) C91(0.5) H91A(0.5) H91B(0.5) C89A(0.5) C78A(0.5)
 C80A(0.5) C79A(0.5) O1B(0.43) C6B(0.43) Cl6(0.5) Cl5(0.5) C92(0.5) H92A(0.5)
 H92B(0.5) P7(0.37) As8(0.21) P6(0.47) As5(0.34) F69B(0.5) F68B(0.5) C88B(0.5)
 C87B(0.5) F64B(0.5) F65B(0.5) O24A(0.5) C84A(0.5) F58A(0.5) F60A(0.5)
 C85A(0.5) F63A(0.5) F62A(0.5) F61A(0.5) C61A(0.75) O23A(0.5) C3B(0.43)
 H3B(0.43) C2B(0.43) H2B(0.43) C1B(0.43) H1B(0.43) C5B(0.43) H5B(0.43)
 C4B(0.43) H4B(0.43) C3A(0.57) H3A(0.57) C4A(0.57) H4A(0.57) C5A(0.57)
 H5A(0.57) C1A(0.57) H1A(0.57) C2A(0.57) H2A(0.57) C62A(0.75) F12A(0.75)
 F10A(0.75) F11A(0.75) C63A(0.75) F14A(0.75) F15A(0.75) F13A(0.75) F59A(0.5)
 C61B(0.25) C62B(0.25) F11B(0.25) F12B(0.25) F10B(0.25) F17B(0.25) F18B(0.25)
 F16B(0.25) C63B(0.25) F15B(0.25) F13B(0.25) F14B(0.25) C58B(0.25) F2B(0.25)
 F3B(0.25) F1B(0.25) C89B(0.5) F1(0.5) F2(0.5) F3(0.5) C88A(0.5) F69A(0.5)
 F68A(0.5) C87A(0.5) F64A(0.5) F65A(0.5) C78B(0.5) F46B(0.5) F47B(0.5)
 F48B(0.5) F53B(0.5) C80B(0.5) F52B(0.5) F50B(0.5) C79B(0.5) F49B(0.5)
 F51B(0.5) C84B(0.5) F58B(0.5) F60B(0.5) F59B(0.5) C85B(0.5) F61B(0.5)
 F62B(0.5) F63B(0.5) O24B(0.5) O23B(0.5) F5B(0.25) C59B(0.25) F4B(0.25)
 C59A(0.75) F4A(0.75) F5A(0.75) C60B(0.25) F7B(0.25) F9B(0.25) F9A(0.75)
 O20A(0.4) C69A(0.4) C70A(0.4) F30A(0.4) F28A(0.4) F29A(0.4) C72A(0.4)
 F35A(0.4) F36A(0.4) F34A(0.4) C71A(0.4) F33A(0.4) F31A(0.4) F32A(0.4)
 O20B(0.24) C69B(0.24) C70B(0.24) F30B(0.24) F28B(0.24) F29B(0.24) C72B(0.24)
 F34B(0.24) F35B(0.24) F36B(0.24) C71B(0.24) F32B(0.24) F33B(0.24) F31B(0.24)
 C57B(0.25) F8B(0.25) O1(0.36) C69C(0.36) C71C(0.36) F33C(0.36) F31C(0.36)
 F32C(0.36) C70C(0.36) F28C(0.36) F29C(0.36) F30C(0.36) C72C(0.36) F36C(0.36)
 F34C(0.36) F35C(0.36)
6.a Secondary CH2 refined with riding coordinates:
 C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B)
6.b Aromatic/amide H refined with riding coordinates:
 C54(H54), C31(H31), C53(H53), C43(H43), C50(H50), C46(H46), C33(H33),
 C30(H30), C45(H45), C51(H51), C44(H44), C23(H23), C32(H32), C8(H8), C47(H47),
 C29(H29), C52(H52), C9(H9), C38(H38), C25(H25), C24(H24), C22(H22), C40(H40),
 C39(H39), C26(H26), C37(H37), C36(H36), C10(H10), C11(H11), C12(H12), C3B(H3B),
  C2B(H2B), C1B(H1B), C5B(H5B), C4B(H4B), C3A(H3A), C4A(H4A), C5A(H5A),
 C1A(H1A), C2A(H2A), C19(H19), C15(H15), C16(H16), C17(H17), C18(H18)
;
_shelx_res_checksum              68066
_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 1.236
_oxdiff_exptl_absorpt_empirical_full_min 0.752