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_7714525
_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 As4 Mo8 O16 P4, 2(Al C16 F36 O4), 2(C H2 Cl2)'
_chemical_formula_sum            'C90 H44 Ag2 Al2 As4 Cl4 F72 Mo8 O24 P4'
_chemical_formula_weight         4479.83
_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             2020-08-26
_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                 91.0400(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.31430(10)
_cell_length_b                   59.1705(3)
_cell_length_c                   21.48980(10)
_cell_measurement_reflns_used    39383
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.4870
_cell_measurement_theta_min      3.6260
_cell_volume                     13113.11(16)
_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  (Sheldrick, 2015)'
_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 0.996
_diffrn_measured_fraction_theta_max 0.980
_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    -27.00  43.00   0.50    5.00    --  -40.03  19.00 -60.00  140
  2  \w      9.00 116.00   0.50    5.00    --   40.03  57.00 -30.00  214
  3  \w     29.00  71.00   0.50   30.00    --  104.85 -61.00 -60.00   84
  4  \w     80.00 178.00   0.50   30.00    --  104.85  77.00 150.00  196
  5  \w     20.00  80.00   0.50   30.00    --  104.85 -95.00  30.00  120
  6  \w     23.00 105.00   0.50   30.00    --  104.85 -77.00-150.00  164
  7  \w     71.00 178.00   0.50   30.00    --  104.85  30.00 -60.00  214
  8  \w     29.00  71.00   0.50   30.00    --  104.85 -61.00  60.00   84
  9  \w     29.00  71.00   0.50   30.00    --  104.85 -61.00  90.00   84
 10  \w     29.00  71.00   0.50   30.00    --  104.85 -61.00  30.00   84
 11  \w     29.00  71.00   0.50   30.00    --  104.85 -61.00 -90.00   84
 12  \w    -98.00 -22.00   0.50    5.00    --  -40.03 125.00  90.00  152
 13  \w      9.00 116.00   0.50    5.00    --   40.03  57.00-150.00  214
 14  \w     71.00 178.00   0.50   30.00    --  104.85  30.00  60.00  214
 15  \w     73.00 152.00   0.50   30.00    --  104.85  61.00-150.00  158
 16  \w     29.00  71.00   0.50   30.00    --  104.85 -61.00 150.00   84
;
_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      -0.1302937000
_diffrn_orient_matrix_UB_12      -0.0008897000
_diffrn_orient_matrix_UB_13      0.0338471000
_diffrn_orient_matrix_UB_21      0.0673278000
_diffrn_orient_matrix_UB_22      -0.0115547000
_diffrn_orient_matrix_UB_23      0.0561357000
_diffrn_orient_matrix_UB_31      0.0284247000
_diffrn_orient_matrix_UB_32      0.0233077000
_diffrn_orient_matrix_UB_33      0.0290907000
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       72
_diffrn_reflns_limit_k_min       -60
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            80363
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.680
_diffrn_reflns_theta_min         3.628
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.401
_exptl_absorpt_correction_T_max  0.360
_exptl_absorpt_correction_T_min  0.034
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.76a (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 dark orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.269
_exptl_crystal_description       block
_exptl_crystal_F_000             8560
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.151
_refine_diff_density_max         1.342
_refine_diff_density_min         -1.701
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2701
_refine_ls_number_reflns         25149
_refine_ls_number_restraints     1082
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+22.9663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1338
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22239
_reflns_number_total             25149
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03490a2.cif
_cod_data_source_block           psh_165_mp_abs_gaus
_cod_database_code               7714525
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C90H40Ag2Al2As4Cl4F73Mo8O25P4
_shelx_estimated_absorpt_t_max   0.256
_shelx_estimated_absorpt_t_min   0.039
_reflns_odcompleteness_completeness 99.60
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 C84B-C81 = C83C-C81
 1.55 with sigma of 0.02
 Cl4B-C90B \\sim Cl4A-C90A \\sim Cl3B-C90B \\sim Cl3A-C90A
 with sigma of 0.02
 F72A-C88A \\sim F70A-C88A \\sim F71A-C88A
 with sigma of 0.02
 C85-C88A \\sim C88B-C85 \\sim C85-C86A \\sim C86B-C85 \\sim C85-C87A \\sim
C87B-C85
 with sigma of 0.02
 F72B-C88B \\sim F70B-C88B \\sim F71B-C88B
 with sigma of 0.02
 F25A-C68A \\sim F27B-C68B \\sim F26B-C68B \\sim F25B-C68B \\sim F26A-C68A
\\sim F27A-C68A \\sim F19B-
 C66B \\sim F20-C66B \\sim F21-C66A \\sim F19A-C66A \\sim F22B-C67B \\sim
F24B-C67B \\sim F23B-C67B ~
 F22A-C67A \\sim F24A-C67A \\sim F23A-C67A
 with sigma of 0.04
 C76B-C73B \\sim C76A-C73A \\sim C74B-C73B \\sim C74A-C73A \\sim C75-C73A \\sim
C75-C73B
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
F64A \\sim F65A \\sim C86A \\sim F66A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
O23A \\sim O23B \\sim O23C \\sim Al2: within 2.1A with sigma of 0.005 and sigma
for terminal atoms of 0.01 within 2.1A
F68B \\sim C87B \\sim F69B \\sim F67B: within 1.9A with sigma of 0.005 and
sigma for terminal atoms of 0.005 within 1.9A
F72A \\sim F70A \\sim F71A \\sim C88A: within 1.9A with sigma of 0.005 and
sigma for terminal atoms of 0.005 within 1.9A
C86A \\sim C86B \\sim C85 \\sim C87A \\sim C87B \\sim C88A \\sim C88B: within
1.9A with sigma of 0.005 and sigma for terminal atoms of 0.005 within 1.9A
F64B \\sim F65B \\sim C86B \\sim F66B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F71B \\sim F72B \\sim C88B \\sim F70B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
C81 \\sim C84C \\sim C83B \\sim C83A \\sim C83C \\sim C82A \\sim C82B \\sim
C82C \\sim C84A \\sim C84B: within 1.9A with sigma of 0.02 and sigma for
terminal atoms of 0.02 within 1.9A
F67A \\sim C87A \\sim F68A \\sim F69A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F58C \\sim F61B \\sim F58A \\sim C83B: within 1.9A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.9A
F60C \\sim F62B \\sim F60A \\sim C84C: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.9A
F56B \\sim F56A \\sim F56C: within 1.9A with sigma of 0.02 and sigma for
terminal atoms of 0.02 within 1.9A
F57B \\sim F62A: within 1.9A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.9A
F40B \\sim F40A \\sim C75 \\sim F41A \\sim F41B: within 1.9A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 1.9A
C4B \\sim C3B \\sim C5B \\sim C7B \\sim C6B \\sim C7A \\sim C3A: within 1.9A
with sigma of 0.02 and sigma for terminal atoms of 0.04 within 1.9A
F17B \\sim C64 \\sim F16B \\sim F16A \\sim F17A \\sim F18 \\sim C61: within
1.9A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
C72B \\sim C72A \\sim C69: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
F33B \\sim F33A \\sim C71A \\sim C71B \\sim F32B \\sim F32A: within 1.9A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
F13A \\sim F13B \\sim C63A \\sim F15A \\sim C63B \\sim F14A \\sim F14B \\sim
F15B \\sim C61: within 1.9A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.9A
F11A \\sim F11B \\sim C62A \\sim C62B \\sim F10A \\sim F10B \\sim F12A \\sim
F12B: within 1.9A with sigma of 0.02 and sigma for terminal atoms of 0.02
within 1.9A
F26B \\sim F23A: within 1.9A with sigma of 0.02 and sigma for terminal atoms of
0.02 within 1.9A
F58B \\sim C83C \\sim F60B \\sim F59B: within 1.9A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.9A
Cl4B \\sim C90B \\sim Cl3B: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.9A
3. Others
 Fixed Sof: Cl4A(0.51) Cl3A(0.51) O18A(0.52) F12A(0.52) F13A(0.52) F32A(0.6)
 F36A(0.5) F16A(0.52) F35A(0.5) F10A(0.52) F33A(0.6) F17A(0.52) O2A(0.59)
 F14A(0.52) F11A(0.52) C6A(0.59) H6A(0.59) C90A(0.51) H90A(0.51) H90B(0.51)
 C2A(0.59) C5A(0.59) H5A(0.59) F15A(0.52) C72A(0.5) C71A(0.6) C7A(0.59)
 H7A(0.59) C63A(0.52) C4A(0.59) H4A(0.59) C62A(0.52) C3A(0.59) H3A(0.59)
 O2B(0.41) C2B(0.41) C6B(0.41) H6B(0.41) C5B(0.41) H5B(0.41) C4B(0.41)
 H4B(0.41) C3B(0.41) H3B(0.41) C7B(0.41) H7B(0.41) C68A(0.52) F26A(0.52)
 F27A(0.52) F25A(0.52) C67A(0.52) F22A(0.52) F23A(0.52) F24A(0.52) C66A(0.52)
 F19A(0.52) C67B(0.48) F23B(0.48) F24B(0.48) F22B(0.48) C68B(0.48) F25B(0.48)
 F26B(0.48) F27B(0.48) C66B(0.48) F19B(0.48) O18B(0.48) F16B(0.48) F17B(0.48)
 C63B(0.48) F14B(0.48) F15B(0.48) F13B(0.48) C62B(0.48) F12B(0.48) F10B(0.48)
 F11B(0.48) O24B(0.46) C86A(0.46) F64A(0.46) F66A(0.46) F65A(0.46) C87A(0.46)
 F69A(0.46) F68A(0.46) F67A(0.46) C88A(0.46) F72A(0.46) F71A(0.46) F70A(0.46)
 C86B(0.54) F66B(0.54) C87B(0.54) F69B(0.54) F68B(0.54) F67B(0.54) C88B(0.54)
 F72B(0.54) F71B(0.54) F70B(0.54) O24A(0.54) F64B(0.54) F65B(0.54) O23A(0.32)
 C84A(0.32) F63A(0.32) F61A(0.32) F62A(0.32) C82A(0.32) F57A(0.32) F56A(0.32)
 F55A(0.32) C83A(0.32) F59A(0.32) F58A(0.32) F60A(0.32) C73B(0.53) F40B(0.53)
 F42B(0.53) F41B(0.53) C76B(0.53) F43B(0.53) F45B(0.53) F44B(0.53) C74B(0.53)
 F37B(0.53) F39B(0.53) F38B(0.53) C73A(0.47) C76A(0.47) F45A(0.47) F44A(0.47)
 F43A(0.47) C74A(0.47) F38A(0.47) F37A(0.47) F39A(0.47) F41A(0.47) F40A(0.47)
 F42A(0.47) F34A(0.5) O23B(0.27) C84C(0.27) F62B(0.27) F61B(0.27) F63B(0.27)
 C82C(0.27) F56B(0.27) F57B(0.27) F55B(0.27) C83C(0.27) F58B(0.27) F60B(0.27)
 F59B(0.27) O23C(0.41) C84B(0.41) F63C(0.41) F61C(0.41) F62C(0.41) C82B(0.41)
 F57C(0.41) F56C(0.41) F55C(0.41) C83B(0.41) F59C(0.41) F58C(0.41) F60C(0.41)
 Cl3B(0.49) C90B(0.49) H90C(0.49) H90D(0.49) Cl4B(0.49) O20B(0.6) O20A(0.4)
 C72B(0.5) F35B(0.5) F34B(0.5) F36B(0.5) F32B(0.4) F33B(0.4) C71B(0.4)
4.a Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C90A(H90A,H90B), C90B(H90C,H90D)
4.b Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C49(H49), C42(H42), C24(H24), C31(H31), C33(H33),
 C11(H11), C41(H41), C47(H47), C38(H38), C56(H56), C46(H46), C48(H48), C19(H19),
  C21(H21), C14(H14), C34(H34), C55(H55), C35(H35), C45(H45), C25(H25),
 C10(H10), C52(H52), C40(H40), C32(H32), C39(H39), C18(H18), C12(H12), C13(H13),
  C53(H53), C17(H17), C20(H20), C26(H26), C6A(H6A), C54(H54), C5A(H5A),
 C7A(H7A), C4A(H4A), C3A(H3A), C6B(H6B), C5B(H5B), C4B(H4B), C3B(H3B), C7B(H7B)
;
_shelx_res_checksum              70167
_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 3.512
_oxdiff_exptl_absorpt_empirical_full_min 0.385