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_7714526
_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
'C28 H20 Ag Mo4 O8 P3.19 Sb0.81, Al C16 F36 O4, 0.45(C H2 Cl2)'
_chemical_formula_sum
'C44.45 H20.9 Ag Al Cl0.9 F36 Mo4 O12 P3.19 Sb0.81'
_chemical_formula_weight         2178.84
_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
_audit_creation_date             2021-03-10
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                106.0900(10)
_cell_angle_beta                 101.8780(10)
_cell_angle_gamma                111.1490(10)
_cell_formula_units_Z            2
_cell_length_a                   14.00870(10)
_cell_length_b                   14.52390(10)
_cell_length_c                   18.68170(10)
_cell_measurement_reflns_used    55855
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.2790
_cell_measurement_theta_min      2.6070
_cell_volume                     3201.62(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (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)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.988
_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     46.00  72.00   0.50    0.05    --   36.00  69.00 -78.41   52
  2  \w     46.00  71.00   0.50    0.05    --   40.00  76.00   6.21   50
  3  \w     59.00  84.00   0.50    0.05    --   48.00  65.00 -54.36   50
  4  \w     61.00  86.00   0.50    0.05    --   48.00  57.00 -30.20   50
  5  \w     61.00  86.00   0.50    0.05    --   48.00  55.00-106.75   50
  6  \w     49.00  74.00   0.50    0.05    --   36.00  55.00-176.54   50
  7  \w     42.00  67.00   0.50    0.05    --   36.00  76.00  88.22   50
  8  \w     50.00  75.00   0.50    0.05    --   40.00  68.00 130.18   50
  9  \w     50.00  77.00   0.50    0.05    --   44.00  77.00  41.42   54
 10  \w     47.00  73.00   0.50    0.05    --   80.00 -82.00   6.09   52
 11  \w     52.00 108.00   0.50    0.05    --   80.00-128.00  36.98  112
 12  \w     42.00 113.00   0.50    0.05    --   80.00-137.00  -5.36  142
 13  \w     42.00  73.00   0.50    0.05    --   80.00-127.00-105.56   62
 14  \w     79.00 105.00   0.50    0.05    --   80.00-127.00-105.56   52
 15  \w     50.00 100.00   0.50    0.05    --   73.72-125.00-120.00  100
 16  \w     56.00 105.00   0.50    0.05    --   80.00-122.00-133.97   98
 17  \w     55.00 103.00   0.50    0.05    --   80.00-119.00-170.53   96
 18  \w     69.00 100.00   0.50    0.05    --   73.72-125.00   0.00   62
 19  \w     74.00 100.00   0.50    0.05    --   80.00-114.00 -64.69   52
 20  \w     39.00  66.00   0.50    0.05    --   80.00-114.00 -64.69   54
 21  \w     74.00  99.00   0.50    0.05    --   80.00-113.00 -10.25   50
 22  \w     52.00 100.00   0.50    0.05    --   80.00-115.00  96.92   96
 23  \w     73.00 100.00   0.50    0.05    --   73.72-125.00 120.00   54
 24  \w     39.00  70.00   0.50    0.05    --   73.72-125.00 120.00   62
 25  \w     41.00  99.00   0.50    0.05    --   80.00-113.00 121.92  116
 26  \w     54.00  98.00   0.50    0.05    --   80.00-113.00  79.33   88
 27  \w     42.00  97.00   0.50    0.05    --   80.00-109.00 139.92  110
 28  \w     43.00  85.00   0.50    0.05    --   80.00-112.00   5.64   84
 29  \w     40.00  66.00   0.50    0.05    --   80.00-112.00  -4.29   52
 30  \w     61.00  94.00   0.50    0.05    --   80.00-112.00-114.87   66
 31  \w     52.00  78.00   0.50    0.05    --   80.00 -88.00 -90.84   52
 32  \w     73.00  98.00   0.50    0.05    --   80.00-112.00  -4.29   50
 33  \w     53.00  92.00   0.50    0.05    --   80.00-108.00  49.18   78
 34  \w     64.00  92.00   0.50    0.05    --   80.00-107.00 171.23   56
 35  \w     42.00  79.00   0.50    0.05    --   80.00-105.00 142.87   74
 36  \w     48.00  73.00   0.50    0.05    --   80.00 -80.00 129.00   50
 37  \w     37.00  62.00   0.50    0.05    --   80.00 -44.00  97.23   50
 38  \w     67.00  93.00   0.50    0.05    --   56.00  65.00  65.46   52
 39  \w     86.00 111.00   0.50    0.05    --   80.00  78.00  60.92   50
 40  \w     71.00  96.00   0.50    0.05    --   60.00  67.00   2.01   50
 41  \w     71.00  96.00   0.50    0.05    --   60.00  65.00 174.66   50
 42  \w     91.00 116.00   0.50    0.05    --   80.00  65.00 171.43   50
 43  \w     92.00 117.00   0.50    0.05    --   80.00  60.00  93.44   50
 44  \w     92.00 118.00   0.50    0.05    --   80.00  58.00  16.94   52
 45  \w     68.00  93.00   0.50    0.05    --   56.00  58.00 -23.78   50
 46  \w     92.00 117.00   0.50    0.05    --   80.00  60.00-107.05   50
 47  \w     92.00 117.00   0.50    0.05    --   80.00  61.00-118.30   50
 48  \w     93.00 118.00   0.50    0.05    --   80.00  47.00-125.12   50
 49  \w     82.00 119.00   0.50    0.05    --   80.00  25.00-169.50   74
 50  \w     59.00  99.00   0.50    0.05    --   66.93  24.00-125.30   80
 51  \w     73.00 105.00   0.50    0.05    --   80.00  24.00-121.66   64
 52  \w     99.00 125.00   0.50    0.05    --   80.00  32.00 -60.30   52
 53  \w     65.00 105.00   0.50    0.05    --   80.00  19.00 -44.07   80
 54  \w     46.00  71.00   0.50    0.05    --   80.00 -74.00 -58.30   50
 55  \w     57.00 121.00   0.50    0.05    --   80.00  12.00-172.42  128
 56  \w     61.00 114.00   0.50    0.05    --   80.00  21.00 120.93  106
 57  \w     62.00 104.00   0.50    0.05    --   66.93  24.00 174.15   84
 58  \w     97.00 122.00   0.50    0.05    --   80.00  17.00  96.72   50
 59  \w     53.00  92.00   0.50    0.05    --   80.00  17.00  96.72   78
 60  \w     63.00 110.00   0.50    0.05    --   80.00  10.00  43.14   94
 61  \w     54.00 116.00   0.50    0.05    --   80.00   4.00 107.40  124
 62  \w     49.00  76.00   0.50    0.05    --   80.00   5.00  34.42   54
 63  \w     39.00 108.00   0.50    0.05    --   73.72   0.00 -30.00  138
 64  \w     76.00 118.00   0.50    0.05    --   80.00   5.00 -37.53   84
 65  \w     59.00  85.00   0.50    0.05    --   80.00   3.00 -99.07   52
 66  \w     49.00  78.00   0.50    0.05    --   80.00   9.00 -77.23   58
 67  \w     84.00 110.00   0.50    0.05    --   80.00   9.00 -77.23   52
 68  \w   -101.00 -76.00   0.50    0.05    --  -77.75 119.00 -24.81   50
 69  \w   -111.00 -86.00   0.50    0.05    --  -77.75 -72.00 -88.24   50
 70  \w   -109.00 -84.00   0.50    0.05    --  -72.00 -65.00  15.57   50
 71  \w   -116.00 -91.00   0.50    0.05    --  -72.00 -40.00  15.95   50
 72  \w   -113.00 -85.00   0.50    0.05    --  -72.00 -51.00 -32.95   56
 73  \w    -81.00 -55.00   0.50    0.05    --  -77.75 116.00-150.05   52
;
_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      -0.0617788000
_diffrn_orient_matrix_UB_12      -0.0057466000
_diffrn_orient_matrix_UB_13      -0.0807702000
_diffrn_orient_matrix_UB_21      0.0836704000
_diffrn_orient_matrix_UB_22      0.1148949000
_diffrn_orient_matrix_UB_23      0.0190152000
_diffrn_orient_matrix_UB_31      0.0701354000
_diffrn_orient_matrix_UB_32      -0.0441817000
_diffrn_orient_matrix_UB_33      -0.0380989000
_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  0.0282
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66769
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.480
_diffrn_reflns_theta_min         2.619
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.051
_exptl_absorpt_correction_T_max  0.706
_exptl_absorpt_correction_T_min  0.054
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (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            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.260
_exptl_crystal_description       block
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         12933
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0255
_refine_ls_R_factor_gt           0.0253
_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^)+(0.0270P)^2^+4.7373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0635
_refine_ls_wR_factor_ref         0.0637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12858
_reflns_number_total             12933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03490a2.cif
_cod_data_source_block           psh_234b_ap_abs_gauss
_cod_original_cell_volume        3201.62(5)
_cod_original_formula_sum
'C44.45 H20.90 Ag Al Cl0.90 F36 Mo4 O12 P3.19 Sb0.81'
_cod_database_code               7714526
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C44.5H21AgAlClF36Mo4O12P3Sb
_reflns_odcompleteness_completeness 98.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-C45 = Cl2-C45
 1.75 with sigma of 0.02
 Ag1-P4 \\sim Ag1-P3
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(P4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.005
4. Others
 Fixed Sof: Cl1(0.45) Cl2(0.45) C45(0.45) H45A(0.45) H45B(0.45) Sb1(0.81)
 C43A(0.77) C44A(0.77) C42A(0.77) F30A(0.77) F33A(0.77) F34A(0.77) F29A(0.77)
 C43B(0.23) C44B(0.23) C42B(0.23) F33B(0.23) F34B(0.23) F35B(0.23) F29B(0.23)
 P4(0.19)
5.a Secondary CH2 refined with riding coordinates:
 C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C14(H14), C3(H3), C11(H11), C7(H7), C12(H12), C13(H13),
 C19(H19), C17(H17), C26(H26), C4(H4), C5(H5), C21(H21), C28(H28), C20(H20),
 C25(H25), C27(H27), C18(H18), C24(H24)
;
_shelx_res_checksum              54994
_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 1.286
_oxdiff_exptl_absorpt_empirical_full_min 0.792