Two in one: a facile modular approach for the assembly of pnictogen-rich heteroleptic organometallic complexes
Mondal, Bijan; Riesinger, Christoph; Scheer, Manfred; Chemical Science  (2025) –; doi:10.1039/D5SC07723K

data_1576221
_publ_section_title
;
 Two in one: a facile modular approach for the assembly of pnictogen-rich
 heteroleptic organometallic complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D5SC07723K
_journal_year                    2025
_chemical_formula_moiety
'C52 H45 Ag2 As6 Fe Mo6 O12 P5, 2(C H2 Cl2), Al C16 F35.675 O4, Al C16 F36 O4, 0.325(F)'
_chemical_formula_sum            'C86 H49 Ag2 Al2 As6 Cl4 F72 Fe Mo6 O20 P5'
_chemical_formula_weight         4417.61
_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             2023-06-02
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.9040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0953(2)
_cell_length_b                   21.5012(2)
_cell_length_c                   31.8903(4)
_cell_measurement_reflns_used    72539
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.5860
_cell_measurement_theta_min      2.4890
_cell_volume                     13076.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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_environment      N~2~
_diffrn_ambient_temperature      123.00(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 0.999
_diffrn_measured_fraction_theta_max 0.979
_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     43.00  79.00   0.30    2.00    --   40.00  73.00 118.00  120
  2  \w     51.00  87.00   0.30    2.00    --   44.00  63.00 159.62  120
  3  \w     11.00  38.90   0.30    2.00    --   60.79 -30.00 -30.00   93
  4  \w   -110.00 -74.00   0.30    2.00    --  -64.00 -52.00 179.42  120
  5  \w   -119.00 -80.00   0.30    2.00    --  -72.00 -47.00 -50.97  130
  6  \w   -119.00 -81.80   0.30    2.00    --  -72.00 -44.00  29.45  124
  7  \w     35.00  84.20   0.30    2.00    --   74.37 -95.00  30.00  164
  8  \w   -114.00 -36.00   0.30    2.00    --  -75.08   0.00  30.00  260
  9  \w     39.00  88.20   0.30    2.00    --   78.43 -95.00 -90.00  164
 10  \w   -120.00 -84.00   0.30    2.00    --  -80.00 -71.00  94.72  120
 11  \w     40.00  80.20   0.30    2.00    --   82.00  -4.00 119.90  134
 12  \w     90.00 126.00   0.30    2.00    --   82.00  56.00 177.40  120
 13  \w     90.00 126.00   0.30    2.00    --   82.00  56.00 -48.36  120
 14  \w     44.00 123.20   0.30    2.00    --   82.00   3.00-153.90  264
 15  \w     64.00 130.00   0.30    2.00    --   82.00  23.00 -63.82  220
 16  \w     52.00 130.00   0.30    2.00    --   82.00  20.00  93.99  260
 17  \w     36.00 108.90   0.30    2.00    --   82.00-119.00 169.53  243
 18  \w     41.00  95.00   0.30    2.00    --   82.00-100.00 173.69  180
 19  \w     39.00  99.00   0.30    2.00    --   82.00-105.00  64.33  200
 20  \w     38.00 117.20   0.30    2.00    --   82.00-134.00 135.32  264
 21  \w     15.00  39.90   0.30    2.00    --   24.00  92.00 -10.63   83
 22  \w     48.00  82.20   0.30    2.00    --   44.00  72.00-118.03  114
 23  \w     11.00  38.90   0.30    2.00    --   60.79 -30.00   0.00   93
 24  \w   -115.00 -77.80   0.30    2.00    --  -68.00 -48.00 -12.01  124
 25  \w    -68.00 -38.00   0.30    2.00    --  -80.00  61.00-108.45  100
 26  \w     40.00  80.20   0.30    2.00    --   82.00  -4.00  70.73  134
 27  \w     38.00  71.00   0.30    2.00    --   82.00 -60.00 -88.77  110
;
_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      0.0725233000
_diffrn_orient_matrix_UB_12      0.0042022000
_diffrn_orient_matrix_UB_13      0.0233192000
_diffrn_orient_matrix_UB_21      0.0210761000
_diffrn_orient_matrix_UB_22      -0.0622995000
_diffrn_orient_matrix_UB_23      -0.0196084000
_diffrn_orient_matrix_UB_31      0.0287326000
_diffrn_orient_matrix_UB_32      0.0351588000
_diffrn_orient_matrix_UB_33      -0.0375431000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_av_unetI/netI     0.0414
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            137288
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.633
_diffrn_reflns_theta_min         2.479
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.427
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.303
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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 red'
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_description       block
_exptl_crystal_F_000             8448
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.164
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2060
_refine_ls_number_reflns         26563
_refine_ls_number_restraints     1005
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1650P)^2^+45.1632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22275
_reflns_number_total             26563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc07723k2.cif
_cod_data_source_block           bm354_cr
_cod_database_code               1576221
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula
'C86  H49  Ag2  Al2  As6  Cl4  F72  Fe  Mo6  O20  P5  '
_shelx_estimated_absorpt_t_max   0.401
_shelx_estimated_absorpt_t_min   0.275
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F44-C65 = F48-C65 = F14-C65
 1.33 with sigma of 0.02
 C47-C3 = C47-C19 = C7-C47
 1.53 with sigma of 0.02
 F15-C7 = F13-C7 = F18-C7 = F4-C3 = F2-C3 = F3-C3 = F5-C19 = F9-C19 = F1-C19
 1.33 with sigma of 0.02
 F83-C54 = F10-C54 = F80-C54 = F44-C65 = F14-C65 = F48-C65 = F22-C66 = F19-C66
 = F7-C66
 1.33 with sigma of 0.02
 C54-C18 = C65-C18 = C66-C18
 1.53 with sigma of 0.02
 F68A-C2
 1.33 with sigma of 0.02
 F68-C108
 1.33 with sigma of 0.02
 F60A-C1 = F69A-C1 = F60-C1
 1.33 with sigma of 0.02
 F63-C112 = F17-C112 = F53-C112
 1.33 with sigma of 0.02
 F107-C106 = F24-C106 = F59-C106
 1.33 with sigma of 0.02
 F41-C140 = F30-C140 = F98-C140
 1.33 with sigma of 0.02
 C91-C120
 1.53 with sigma of 0.02
 F83A-C54A = F80A-C54A = F10A-C54A
 1.33 with sigma of 0.02
 C55-C140
 1.53 with sigma of 0.02
 F32A-C71A = F6A-C71A = F36A-C71A
 1.33 with sigma of 0.02
 F44-F48
 2.2 with sigma of 0.04
 F48-F14
 2.2 with sigma of 0.04
 C3-C19
 2.55 with sigma of 0.04
 C19-C7
 2.55 with sigma of 0.04
 C7-C3
 2.55 with sigma of 0.04
 F13-F15
 2.2 with sigma of 0.04
 F15-F18
 2.2 with sigma of 0.04
 F18-F13
 2.2 with sigma of 0.04
 F4-F2
 2.2 with sigma of 0.04
 F2-F3
 2.2 with sigma of 0.04
 F3-F4
 2.2 with sigma of 0.04
 F9-F5
 2.2 with sigma of 0.04
 F5-F1
 2.2 with sigma of 0.04
 F1-F9
 2.2 with sigma of 0.04
 C54-C65
 2.55 with sigma of 0.04
 C65-C66
 2.55 with sigma of 0.04
 C66-C54
 2.55 with sigma of 0.04
 F14-F44
 2.2 with sigma of 0.04
 F10-F83
 2.2 with sigma of 0.04
 F83-F80
 2.2 with sigma of 0.04
 F80-F10
 2.2 with sigma of 0.04
 F60-F60A
 2.2 with sigma of 0.04
 F60-F69A
 2.2 with sigma of 0.04
 F69A-F60A
 2.2 with sigma of 0.04
 F53-F63
 2.2 with sigma of 0.04
 F53-F17
 2.2 with sigma of 0.04
 F17-F63
 2.2 with sigma of 0.04
 F107-F59
 2.2 with sigma of 0.04
 F59-F24
 2.2 with sigma of 0.04
 F24-F107
 2.2 with sigma of 0.04
 F41-F30
 2.2 with sigma of 0.04
 F30-F98
 2.2 with sigma of 0.04
 F98-F41
 2.2 with sigma of 0.04
 F80A-F83A
 2.2 with sigma of 0.04
 F83A-F10A
 2.2 with sigma of 0.04
 F10A-F80A
 2.2 with sigma of 0.04
 F6A-F32A
 2.2 with sigma of 0.04
 F32A-F36A
 2.2 with sigma of 0.04
 F36A-F6A
 2.2 with sigma of 0.04
 F80-F83 \\sim F80A-F83A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O3 \\sim F7 \\sim F10 \\sim F14 \\sim C18 \\sim F19 \\sim F22 \\sim F39 \\sim
F44 \\sim F48 \\sim C54 \\sim C65 \\sim C66 \\sim F80 \\sim F83 \\sim O3A \\sim
F7A \\sim F10A \\sim F14A \\sim F19A \\sim F22A \\sim F44A \\sim F48A \\sim
C54A \\sim C65A \\sim C66A \\sim F80A \\sim F83A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
F6 \\sim F21 \\sim F32 \\sim C34 \\sim F36 \\sim F43 \\sim F60 \\sim F68 \\sim
F69 \\sim C71 \\sim F85 \\sim C100 \\sim C108 \\sim F6A \\sim F21A \\sim F32A
\\sim F36A \\sim F60A \\sim F68A \\sim F69A \\sim C71A \\sim F85A \\sim C1
\\sim C2: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 1.7A
F16 \\sim F17 \\sim F20 \\sim F30 \\sim F33 \\sim F41 \\sim F53 \\sim C55 \\sim
F63 \\sim F98 \\sim C112 \\sim C115 \\sim C140: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
F52 \\sim F56 \\sim F70 \\sim F73 \\sim F86 \\sim F88 \\sim C91 \\sim C94 \\sim
F96 \\sim F101 \\sim C110 \\sim C120 \\sim F42: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 1.7A
C47 \\sim F3 \\sim F4 \\sim F5 \\sim F13 \\sim F9 \\sim F1 \\sim F2 \\sim F15
\\sim C3 \\sim F18 \\sim C7 \\sim C19: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F39 \\sim C50 \\sim F51 \\sim F59 \\sim F61 \\sim F64 \\sim F95 \\sim F105
\\sim C106 \\sim F107 \\sim C113 \\sim C124 \\sim F24: within 1.7A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
4. Others
 Sof(F14)=Sof(F44)=Sof(F48)=Sof(C65)=Sof(O3A)=Sof(F7A)=Sof(F10A)=Sof(F19A)=
 Sof(F22A)=Sof(C54A)=Sof(C66A)=Sof(F80A)=Sof(F83A)=1-FVAR(1)
 Sof(O3)=Sof(F7)=Sof(F10)=Sof(F19)=Sof(F22)=Sof(C54)=Sof(C66)=Sof(F80)=
 Sof(F83)=Sof(F14A)=Sof(F44A)=Sof(F48A)=Sof(C65A)=FVAR(1)
 Sof(F6A)=Sof(F21A)=Sof(F32A)=Sof(F36A)=Sof(F60A)=Sof(F68A)=Sof(F69A)=
 Sof(C71A)=Sof(F85A)=Sof(C1)=Sof(C2)=1-FVAR(2)
 Sof(F6)=Sof(F21)=Sof(F32)=Sof(F36)=Sof(F43)=Sof(F68)=Sof(F69)=Sof(C71)=
 Sof(F85)=Sof(C100)=Sof(C108)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C04T(H04E,H04F), C05G(H05A,H05B)
5.b Aromatic/amide H refined with riding coordinates:
 C025(H025), C02A(H02A), C02M(H02M), C02P(H02P), C02R(H02R), C02S(H02S),
 C02T(H02T), C02U(H02U), C02Y(H02Y), C02Z(H02Z), C032(H032), C034(H034),
 C038(H038), C039(H039), C03A(H03D), C03F(H03F), C03G(H03G), C03I(H03I),
 C03J(H03J), C03M(H03M), C03N(H03N), C03P(H03P), C03R(H03R), C03W(H03W),
 C03X(H03X), C041(H041), C043(H043), C04A(H04D), C04G(H04G), C04K(H04K)
5.c Idealised Me refined as rotating group:
 C01Y(H01A,H01B,H01C), C02F(H02B,H02C,H02D), C02W(H02E,H02F,H02G), C030(H03A,
 H03B,H03C), C045(H04A,H04B,H04C)
;
_shelx_res_checksum              83829
_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 2.237
_oxdiff_exptl_absorpt_empirical_full_min 0.557