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_7714529
_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 Cu Mo4 O8 P3.08 Sb0.92, Al C16 F36 O4, C7 H8'
_chemical_formula_sum            'C51 H28 Al Cu F36 Mo4 O12 P3.08 Sb0.92'
_chemical_formula_weight         2198.41
_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
_audit_creation_date             2021-04-30
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2021.04.28 svn.r794ee209 for OlexSys, GUI svn.r6317)
;
_audit_update_record
;
2023-10-12 deposited with the CCDC.	2023-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.768(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.6787(3)
_cell_length_b                   23.0865(3)
_cell_length_c                   19.1437(3)
_cell_measurement_reflns_used    35676
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      33.9650
_cell_measurement_theta_min      3.0360
_cell_volume                     6845.7(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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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    -23.00   2.00   1.00   14.77    --   23.58 -56.00 138.00   25
  2  \w     -3.00  45.00   1.00   14.77    --   23.58  56.00 -79.00   48
  3  \w    -95.00   4.00   1.00   14.77    --  -23.73 -56.00 138.00   99
  4  \w     -2.00  31.00   1.00   14.77    --  -23.73  56.00 -79.00   33
  5  \w     -9.00  41.00   1.00   14.77    --   23.58  77.00 150.00   50
  6  \w     74.00 100.00   1.00   14.77    --   23.58 178.00-180.00   26
  7  \w     -9.00  42.00   1.00   14.77    --   23.58  77.00 -30.00   51
  8  \w    -98.00  -1.00   1.00   14.77    --  -23.73 -38.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0250183000
_diffrn_orient_matrix_UB_12      0.0179876000
_diffrn_orient_matrix_UB_13      -0.0302810000
_diffrn_orient_matrix_UB_21      -0.0232647000
_diffrn_orient_matrix_UB_22      0.0103301000
_diffrn_orient_matrix_UB_23      0.0218416000
_diffrn_orient_matrix_UB_31      0.0304822000
_diffrn_orient_matrix_UB_32      0.0226759000
_diffrn_orient_matrix_UB_33      0.0140704000
_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  0.0266
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            85359
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.998
_diffrn_reflns_theta_min         2.602
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.505
_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            'intense red'
_exptl_crystal_density_diffrn    2.133
_exptl_crystal_description       block
_exptl_crystal_F_000             4228
_exptl_crystal_size_max          0.308
_exptl_crystal_size_mid          0.257
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.283
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2010
_refine_ls_number_reflns         21810
_refine_ls_number_restraints     1275
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0374
_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^)+(0.0223P)^2^+10.8019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0799
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17954
_reflns_number_total             21810
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03490a2.cif
_cod_data_source_block           psh224_mo_mp_abs
_cod_database_code               7714529
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C51H28AlCuF36Mo4O12P3.1Sb0.9
_shelx_estimated_absorpt_t_max   0.728
_shelx_estimated_absorpt_t_min   0.636
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.93
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C46B-C47B = C47B-C48B = C48B-C49B = C49B-C50B = C50B-C51B = C51B-C46B
 1.35 with sigma of 0.02
 C45A-C46A = C46B-C45B
 1.54 with sigma of 0.02
 F8C-C32C \\sim F9C-C32C \\sim F7C-C32C \\sim F4C-C31C \\sim F5C-C31C \\sim
F3C-C30C \\sim F1C-C30C ~
 F2C-C30C
 with sigma of 0.04
 C33A-C36A \\sim C33A-C36C \\sim C33A-C34C \\sim C34A-C33A \\sim C33A-C35C
\\sim C35A-C33A
 with sigma of 0.02
 C45B-C51B \\sim C45B-C47B
 with sigma of 0.04
 C46B-C50B \\sim C46B-C48B \\sim C51B-C49B \\sim C47B-C51B \\sim C48B-C50B
\\sim C47B-C49B
 with sigma of 0.04
 F1B-C30B \\sim F2B-C30B \\sim F3B-C30B \\sim F8B-C32B \\sim F9B-C32B \\sim
F7B-C32B \\sim F6B-C31B ~
 F4B-C31B
 with sigma of 0.04
 C29C-C32C \\sim C29C-C31C \\sim C29C-C30C
 with sigma of 0.04
 F8A-C32A \\sim F9A-C32A \\sim F7A-C32A \\sim F4A-C31A \\sim F5A-C31A \\sim
F6A-C31A \\sim F3A-C30A ~
 F1A-C30A \\sim F2A-C30A
 with sigma of 0.04
 C29A-C32A \\sim C29A-C31A \\sim C29A-C30A
 with sigma of 0.04
 C29B-C30B \\sim C29B-C32B \\sim C29B-C31B
 with sigma of 0.04
 F22C-F23C \\sim F23C-F24C \\sim F24C-F22C
 with sigma of 0.02
 F19C-C38C \\sim F20C-C38C \\sim F21C-C38C \\sim F24C-C39C \\sim F22C-C39C
\\sim F23C-C39C \\sim F25C-
 C40C \\sim F26C-C40C \\sim F27C-C40C
 with sigma of 0.02
 C37-C39A \\sim C38B-C37 \\sim C37-C40A \\sim C39B-C37 \\sim C37-C38A \\sim
C40B-C37
 with sigma of 0.01
 F21B-F19B \\sim F19B-F20B \\sim F20B-F21B
 with sigma of 0.02
 F22B-C39B \\sim F23B-C39B \\sim F24B-C39B \\sim F25B-C40B \\sim F26B-C40B
\\sim F27B-C40B \\sim F19B-
 C38B \\sim F20B-C38B \\sim F21B-C38B
 with sigma of 0.02
 F18A-F16A \\sim F16A-F17A \\sim F17A-F18A
 with sigma of 0.01
 F15A-C35A \\sim F15C-C35A \\sim F15C-C35C \\sim F15A-C35C \\sim F14A-C35A
 with sigma of 0.02
3. Restrained planarity
 C50B, C45B, C46B, C47B, C51B, C48B, C49B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
C36A \\sim C36C \\sim C33A \\sim C35C \\sim C35A \\sim C34A \\sim C34C: within
1.7A with sigma of 0.02 and sigma for terminal atoms of 0.02 within 1.7A
C45A \\sim C45B \\sim C46A \\sim C47B \\sim C47A \\sim C48A \\sim C48B \\sim
C49B \\sim C49A \\sim C50B \\sim C50A \\sim C51B \\sim C51A \\sim C46B: within
1.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.8A
C44C \\sim F36C \\sim F35C \\sim F34C: within 1.8A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.8A
F5C \\sim C31C \\sim F4C: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.01 within 1.7A
C39C \\sim F22C \\sim F24C \\sim F23C: within 1.8A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.8A
C37 \\sim C39A \\sim C39C \\sim C38B \\sim C38C \\sim C40B \\sim C38A \\sim
C39B \\sim C40C \\sim C40A: within 1.8A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.8A
C29A \\sim C29B \\sim C29C \\sim C30B \\sim C30C \\sim C30A \\sim C32B \\sim
C32C \\sim C32A \\sim C31B \\sim C31C \\sim C31A: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 1.7A
C31B \\sim F6B \\sim F4B \\sim F5B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F7C \\sim C32C \\sim F8C \\sim F9C: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F2C \\sim F3C \\sim C30C \\sim F1C: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F9B \\sim C32B \\sim F8B \\sim F7B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
C37 \\sim C40B \\sim C39A \\sim C38B \\sim C40A \\sim C38A \\sim C39B: within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01 within 1.7A
O9A \\sim O9B \\sim Al1: within 1.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.8A
F22B \\sim F25C \\sim C40C \\sim C39B \\sim F23B \\sim F26C \\sim F27C \\sim
F24B: within 1.8A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 1.8A
C44C \\sim C44A \\sim C41A \\sim C43C: within 1.8A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.8A
F32C \\sim C43C \\sim F33C \\sim F31C: within 1.8A with sigma of 0.02 and sigma
for terminal atoms of 0.02 within 1.8A
F21B \\sim C38B \\sim F19B \\sim F20B: within 1.7A with sigma of 0.005 and
sigma for terminal atoms of 0.005 within 1.7A
F25B \\sim C40B \\sim F27B \\sim F26B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
F20C \\sim C38C \\sim F21C \\sim F19C: within 1.8A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.8A
F15C \\sim C35C \\sim F15A \\sim C35A \\sim F14A \\sim F14C: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
O10A \\sim O10B \\sim Al1: within 1.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 1.8A
C5B \\sim C4A \\sim C1B \\sim C3A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.04 within 1.7A
F36A \\sim C44A \\sim F34A \\sim F35A: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.7A
F13C \\sim F13A \\sim F15C \\sim C35A \\sim C35C \\sim F15A: within 1.7A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
5. Others
 Fixed Sof: Sb2(0.46) Sb1(0.46) O2A(0.67) O11A(0.67) F21A(0.62) F26A(0.62)
 F20A(0.62) F27A(0.62) C3A(0.67) H3A(0.67) C7A(0.67) F19A(0.62) C4A(0.67)
 H4A(0.67) O1A(0.67) F23A(0.62) F25A(0.62) F22A(0.62) C1A(0.67) H1A(0.67)
 C6A(0.67) C5A(0.67) H5A(0.67) C46A(0.8) C47A(0.8) H47A(0.8) C2A(0.67)
 H2A(0.67) C40A(0.62) C48A(0.8) H48A(0.8) C38A(0.62) C51A(0.8) H51A(0.8)
 C45A(0.8) H45A(0.8) H45B(0.8) H45C(0.8) C39A(0.62) C50A(0.8) H50A(0.8)
 C49A(0.8) H49A(0.8) O10A(0.64) C33A(0.64) C35A(0.31) F14A(0.31) F15A(0.31)
 C34A(0.31) F10A(0.31) F11A(0.31) F12A(0.64) C36A(0.31) F18A(0.31) F16A(0.64)
 F17A(0.31) O12A(0.7) C41A(0.7) C43A(0.49) F32A(0.49) F33A(0.49) F31A(0.49)
 C42A(0.7) F30A(0.7) F28A(0.7) F29A(0.7) C44A(0.49) F36A(0.49) F34A(0.49)
 F35A(0.49) O12B(0.3) C41B(0.3) C42B(0.3) F29B(0.3) F30B(0.3) F28B(0.3)
 C44B(0.3) F34B(0.3) F35B(0.3) F36B(0.3) C43B(0.3) F32B(0.3) F33B(0.3)
 F31B(0.3) C29A(0.4) C32A(0.4) F8A(0.4) F9A(0.4) F7A(0.4) C31A(0.4) F4A(0.4)
 F5A(0.4) F6A(0.68) C30A(0.4) F3A(0.4) F1A(0.4) F2A(0.4) O10B(0.36) C33B(0.36)
 C35B(0.36) F15B(0.36) F13B(0.36) F14B(0.36) C34B(0.36) F11B(0.36) F12B(0.36)
 F10B(0.36) C36B(0.36) F18B(0.36) F16B(0.36) F17B(0.36) C38B(0.21) F21B(0.21)
 F19B(0.21) F20B(0.21) C40B(0.21) F26B(0.21) F27B(0.83) F25B(0.21) C39B(0.21)
 F24B(0.21) F22B(0.21) F23B(0.21) O9B(0.32) C29B(0.32) C30B(0.32) F1B(0.32)
 F2B(0.32) F3B(0.32) C32B(0.32) F8B(0.32) F9B(0.32) F7B(0.32) C31B(0.32)
 F6B(0.32) F4B(0.32) O1B(0.33) C6B(0.33) C1B(0.33) H1B(0.33) C5B(0.33)
 H5B(0.33) C4B(0.33) H4B(0.33) C2B(0.33) H2B(0.33) C3B(0.33) H3B(0.33)
 C7B(0.33) O2B(0.33) P3(0.54) P4(0.54) F5B(0.32) O9A(0.68) C29C(0.28)
 C32C(0.28) F8C(0.28) F9C(0.28) F7C(0.28) C31C(0.28) F4C(0.28) F5C(0.28)
 C30C(0.28) F3C(0.28) F1C(0.28) F2C(0.28) C35C(0.33) F15C(0.33) F14C(0.33)
 C34C(0.33) F10C(0.33) F11C(0.33) C36C(0.33) F17C(0.33) F16C(0.33) C45B(0.2)
 H45D(0.2) H45E(0.2) H45F(0.2) C46B(0.2) C47B(0.2) H47B(0.2) C48B(0.2)
 H48B(0.2) C49B(0.2) H49B(0.2) C50B(0.2) H50B(0.2) C51B(0.2) H51B(0.2)
 C43C(0.21) F32C(0.21) F33C(0.21) F31C(0.21) C44C(0.21) F36C(0.21) F34C(0.21)
 F35C(0.21) O11B(0.33) C40C(0.17) F27C(0.17) F25C(0.17) F26C(0.17) C39C(0.17)
 F22C(0.17) F23C(0.17) F24C(0.17) C38C(0.17) F21C(0.17) F19C(0.17) F20C(0.17)
 F13A(0.31) F13C(0.33)
6.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C19(H19), C17(H17), C18(H18), C15(H15), C16(H16), C26(H26),
 C24(H24), C4A(H4A), C25(H25), C22(H22), C23(H23), C11(H11), C12(H12), C1A(H1A),
  C8(H8), C10(H10), C5A(H5A), C9(H9), C47A(H47A), C2A(H2A), C48A(H48A),
 C51A(H51A), C50A(H50A), C49A(H49A), C1B(H1B), C5B(H5B), C4B(H4B), C2B(H2B),
 C3B(H3B), C47B(H47B), C48B(H48B), C49B(H49B), C50B(H50B), C51B(H51B)
6.b Idealised Me refined as rotating group:
 C45A(H45A,H45B,H45C), C45B(H45D,H45E,H45F)
;
_shelx_res_checksum              28815
_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 1.066
_oxdiff_exptl_absorpt_empirical_full_min 0.942