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_1576220
_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
'C48 H50 Ag2 Fe2 Mo4 O8 P14, 2(Al C16 F36 O4), 1.16(C H2 Cl2)'
_chemical_formula_sum
'C81.16 H52.32 Ag2 Al2 Cl2.32 F72 Fe2 Mo4 O16 P14'
_chemical_formula_weight         3932.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2025-06-22 deposited with the CCDC.	2025-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                103.8920(10)
_cell_angle_beta                 103.6720(10)
_cell_angle_gamma                112.409(2)
_cell_formula_units_Z            2
_cell_length_a                   18.5453(3)
_cell_length_b                   19.3393(4)
_cell_length_c                   21.2202(3)
_cell_measurement_reflns_used    29494
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.8890
_cell_measurement_theta_min      2.1320
_cell_volume                     6358.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_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      100.01(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 0.866
_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    -58.00  16.00   0.50   50.00    --    2.54 -58.00  88.00  148
  2  \w    -11.00  63.00   0.50   50.00    --    2.54  58.00-130.00  148
  3  \w    -16.00  57.00   0.50   50.00    --   -3.16  58.00-130.00  146
  4  \w    -63.00  10.00   0.50   50.00    --   -3.16 -58.00  88.00  146
  5  \w    -10.00  63.00   0.50   50.00    --    2.54  57.00   0.00  146
  6  \w    -50.00  23.00   0.50   50.00    --    2.54 -77.00  60.00  146
  7  \w    -50.00  23.00   0.50   50.00    --    2.54 -77.00   0.00  146
  8  \w    -18.00  31.00   0.50   50.00    --   -3.16 -99.00 -30.00   98
  9  \w    -63.00 -38.00   0.50   50.00    --    2.54 -38.00 -90.00   50
 10  \w    -18.00  37.00   0.50   50.00    --    2.54 -99.00-180.00  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      -0.0391475000
_diffrn_orient_matrix_UB_12      -0.0323174000
_diffrn_orient_matrix_UB_13      -0.0239521000
_diffrn_orient_matrix_UB_21      -0.0202752000
_diffrn_orient_matrix_UB_22      0.0232362000
_diffrn_orient_matrix_UB_23      0.0092364000
_diffrn_orient_matrix_UB_31      0.0056233000
_diffrn_orient_matrix_UB_32      0.0153447000
_diffrn_orient_matrix_UB_33      -0.0266317000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            39759
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.894
_diffrn_reflns_theta_min         1.893
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       needle
_exptl_crystal_F_000             3809
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.028
_refine_diff_density_max         2.078
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1902
_refine_ls_number_reflns         39759
_refine_ls_number_restraints     273
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0986P)^2^+30.7971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                30669
_reflns_number_total             39759
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9928\% 
around [-0.71 0.71 -0.00] (reciprocal) or [-0.76 0.65 -0.01] (direct)
;
_cod_data_source_file            d5sc07723k2.cif
_cod_data_source_block           bm120_ap_abs_gaus_twin1_hklf5
_cod_database_code               1576220
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C81.2H52.3Ag2Al2Cl2.3F72Fe2Mo4O16P14
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.780
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5314(8)
 0.4686(8)
2. 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
3. Restrained distances
 Cl3-C82 = Cl4-C82
 1.77 with sigma of 0.02
 Cl3-Cl4
 2.9 with sigma of 0.04
 F9B-C52B \\sim F8B-C52B \\sim F7B-C52B \\sim F1B-C50B \\sim F2B-C50B \\sim
F3B-C50B \\sim F4B-C51B ~
 F5B-C51B \\sim F6B-C51B
 with sigma of 0.02
 F8B-F9B \\sim F9B-F7B \\sim F7B-F8B
 with sigma of 0.02
 C50B-C49 \\sim C50A-C49 \\sim C51B-C49 \\sim C51A-C49 \\sim C52B-C49 \\sim
C52A-C49
 with sigma of 0.02
 F5A-C51A \\sim F6A-C51A \\sim F4A-C51A \\sim F8A-C52A \\sim F9A-C52A \\sim
F7A-C52A \\sim F1A-C50A ~
 F2A-C50A \\sim F3A-C50A
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
F5A \\sim F4A \\sim F6A \\sim C51A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C52B \\sim F8B \\sim F9B \\sim F7B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C52A \\sim F8A \\sim F7A \\sim F9A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F2B \\sim C50B \\sim F1B \\sim F3B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F2A \\sim F1A \\sim C50A \\sim F3A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
C49 \\sim C51B \\sim C51A \\sim C52A \\sim C52B \\sim C50A \\sim C50B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
F5B \\sim C51B \\sim F6B \\sim F4B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
Uanis(Cl4) \\sim Ueq, Uanis(C82) \\sim Ueq, Uanis(Cl3) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
5. Others
 Fixed Sof: F8A(0.56) F5A(0.56) F3A(0.56) F2A(0.56) F7A(0.56) F1A(0.56)
 F9A(0.56) F6A(0.56) F4A(0.56) C52A(0.56) C51A(0.56) C50A(0.56) Cl3(0.16)
 Cl4(0.16) C82(0.16) H82A(0.16) H82B(0.16) C52B(0.44) F8B(0.44) F9B(0.44)
 F7B(0.44) C51B(0.44) F6B(0.44) F5B(0.44) F4B(0.44) F1B(0.44) F3B(0.44)
 C50B(0.44) F2B(0.44)
6.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C82(H82A,H82B)
6.b Aromatic/amide H refined with riding coordinates:
 C33(H33), C32(H32), C47(H47), C23(H23), C27(H27), C46(H46), C40(H40),
 C31(H31), C37(H37), C38(H38), C41(H41), C45(H45), C26(H26), C39(H39), C34(H34),
  C48(H48), C30(H30), C24(H24), C44(H44), C25(H25)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C20(H20A,H20B,H20C),
 C18(H18A,H18B,H18C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
  C19(H19A,H19B,H19C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              18642
_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 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.683
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2