Supramolecular compounds assembled from the heteroleptic tetrahedral complex [{CpMo(CO)<sub>2</sub>}<sub>2</sub>(μ,η<sup>2</sup>-AsSb)] and metal salts.
Elsayed Moussa, Mehdi; Shelyganov, Pavel A.; Seidl, Michael; Zimmermann, Lisa; Scheer, Manfred; Chemical communications (Cambridge, England) 60 (2024) 4703–4706; doi:10.1039/d4cc01001a

data_7132923
_publ_section_title
;
 Supramolecular compounds assembled from the heteroleptic tetrahedral
 complex
 [{CpMo(CO)<sub>2</sub>}<sub>2</sub>(&#x3bc;,&#x3b7;<sup>2</sup>-AsSb)]
 and metal salts.
;
_journal_issue                   35
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4703
_journal_page_last               4706
_journal_paper_doi               10.1039/d4cc01001a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'C33.12 H27.68 As2 Cu2 Mo4 N2.56 O8 Sb2, 2(Al C36 F46 O3), 0.44(C2 H3 N1), C H2 Cl2, 1.8[CH2Cl2]'
_chemical_formula_sum
'C108.8 H34.6 Al2 As2 Cl5.6 Cu2 F92 Mo4 N3 O14 Sb2'
_chemical_formula_weight         4512.25
_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
_audit_creation_date             2024-03-28
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-03-28 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.5123(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6343(3)
_cell_length_b                   19.0078(2)
_cell_length_c                   31.4538(3)
_cell_measurement_reflns_used    41121
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.0650
_cell_measurement_theta_min      3.6290
_cell_volume                     13974.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (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_temperature      123.01(10)
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.959
_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   -116.00 -23.00   0.50    5.00    --  -45.40 -37.00 -30.00  186
  2  \w     17.00 121.00   0.50    5.00    --   45.40  19.00 -90.00  208
  3  \w     36.00  72.00   0.50   20.00    --  104.50 -45.00 -90.00   72
  4  \w    103.00 176.00   0.50   20.00    --  104.50  77.00 -60.00  146
  5  \w     35.00  93.00   0.50   20.00    --  104.50 -61.00-180.00  116
  6  \w     97.00 176.00   0.50   20.00    --  104.50 125.00  60.00  158
  7  \w     35.00  93.00   0.50   20.00    --  104.50 -61.00  60.00  116
  8  \w     97.00 176.00   0.50   20.00    --  104.50 125.00  30.00  158
  9  \w    103.00 176.00   0.50   20.00    --  104.50  77.00-180.00  146
 10  \w     -5.00  30.00   0.50    5.00    --  -45.40  19.00 150.00   70
 11  \w   -115.00 -21.00   0.50    5.00    --  -45.40 -57.00  90.00  188
 12  \w    -30.00  48.00   0.50    5.00    --   45.40 -19.00 -90.00  156
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            77578
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.554
_diffrn_reflns_theta_min         3.435
_exptl_absorpt_coefficient_mu    9.523
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.013
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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    2.145
_exptl_crystal_description       plate
_exptl_crystal_F_000             8654
_exptl_crystal_size_max          0.67
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.668
_refine_diff_density_min         -1.940
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2399
_refine_ls_number_reflns         27430
_refine_ls_number_restraints     665
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0716
_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^)+(0.0799P)^2^+96.7712P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1842
_refine_ls_wR_factor_ref         0.1875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25179
_reflns_number_total             27430
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01001a2.cif
_cod_data_source_block           psh_132_mp_testabs
_cod_depositor_comments
'Adding full bibliography for 7132918--7132923.cif.'
_cod_original_formula_sum
'C108.80 H34.60 Al2 As2 Cl5.60 Cu2 F92 Mo4 N3 O14 Sb2'
_cod_database_code               7132923
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.555
_shelx_estimated_absorpt_t_min   0.061
_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
 Sb2-As7
 2.7 with sigma of 0.02
 Sb2C-As2C
 2.7 with sigma of 0.02
 As2B-Mo3B
 2.65 with sigma of 0.02
 C25A-C26A \\sim C26B-C25B \\sim C27A-C26A \\sim C26B-C27B \\sim C28B-C27B
\\sim C28A-C27A \\sim C24A-
 C28A \\sim C28B-C24B \\sim C24B-C25B \\sim C24A-C25A
 with sigma of 0.02
 Sb2A-As2A \\sim Sb2B-As2B
 with sigma of 0.01
 Mo4B-C22B \\sim Mo4A-C22A
 with sigma of 0.02
 O7B-C22B \\sim O7A-C22A
 with sigma of 0.02
 Sb1B-As1B \\sim Sb1A-As1A
 with sigma of 0.01
 As2B-Cu11 \\sim As2C-Cu11
 with sigma of 0.02
 Sb2B-Cu1 \\sim Sb2C-Cu1
 with sigma of 0.02
 Sb2B-Cu10 \\sim Sb2C-Cu10
 with sigma of 0.02
 C20B-Mo3B \\sim C20B-Mo3C
 with sigma of 0.02
 C19B-Mo3B \\sim C19B-Mo3C
 with sigma of 0.02
 C18B-Mo3B \\sim C18B-Mo3C
 with sigma of 0.02
 C17B-Mo3B \\sim C17B-Mo3C
 with sigma of 0.02
 C21B-Mo3B \\sim C21B-Mo3C
 with sigma of 0.02
 Mo3B-C16B \\sim Mo3C-C16B
 with sigma of 0.02
 C22B-Mo4B \\sim C22B-Mo4C
 with sigma of 0.02
 Mo4B-C25B \\sim Mo4C-C25B
 with sigma of 0.02
 Mo4B-C26B \\sim Mo4C-C26B
 with sigma of 0.02
 Mo4B-C27B \\sim Mo4C-C27B
 with sigma of 0.02
 Mo4B-C28B \\sim Mo4C-C28B
 with sigma of 0.02
 Mo4B-C24B \\sim Mo4C-C24B
 with sigma of 0.02
 As2B-Sb2B \\sim As2C-Sb2C
 with sigma of 0.04
 As2B-Cu2 \\sim As2C-Cu2
 with sigma of 0.04
 As2B-Cu1 \\sim As2C-Cu1
 with sigma of 0.04
 As2B-Mo3B \\sim As2C-Mo3C
 with sigma of 0.04
 As2B-C22B \\sim As2C-C22B
 with sigma of 0.04
 As2B-Mo4B \\sim As2C-Mo4C
 with sigma of 0.04
 As2B-C25B \\sim As2C-C25B
 with sigma of 0.04
 As2B-C26B \\sim As2C-C26B
 with sigma of 0.04
 As2B-C27B \\sim As2C-C27B
 with sigma of 0.04
 As2B-C28B \\sim As2C-C28B
 with sigma of 0.04
 As2B-C24B \\sim As2C-C24B
 with sigma of 0.04
 As2B-Cu10 \\sim As2C-Cu10
 with sigma of 0.04
 Sb2B-Cu2 \\sim Sb2C-Cu2
 with sigma of 0.04
 Sb2B-C20B \\sim Sb2C-C20B
 with sigma of 0.04
 Sb2B-C19B \\sim Sb2C-C19B
 with sigma of 0.04
 Sb2B-C18B \\sim Sb2C-C18B
 with sigma of 0.04
 Sb2B-C17B \\sim Sb2C-C17B
 with sigma of 0.04
 Sb2B-C21B \\sim Sb2C-C21B
 with sigma of 0.04
 Sb2B-Mo3B \\sim Sb2C-Mo3C
 with sigma of 0.04
 Sb2B-C16B \\sim Sb2C-C16B
 with sigma of 0.04
 Sb2B-C22B \\sim Sb2C-C22B
 with sigma of 0.04
 Sb2B-Mo4B \\sim Sb2C-Mo4C
 with sigma of 0.04
 Sb2B-C25B \\sim Sb2C-C25B
 with sigma of 0.04
 Sb2B-C26B \\sim Sb2C-C26B
 with sigma of 0.04
 Sb2B-C27B \\sim Sb2C-C27B
 with sigma of 0.04
 Sb2B-C28B \\sim Sb2C-C28B
 with sigma of 0.04
 Sb2B-C24B \\sim Sb2C-C24B
 with sigma of 0.04
 Sb2B-Cu11 \\sim Sb2C-Cu11
 with sigma of 0.04
 Cu2-Mo3B \\sim Cu2-Mo3C
 with sigma of 0.04
 Cu2-Mo4B \\sim Cu2-Mo4C
 with sigma of 0.04
 Cu1-Mo3B \\sim Cu1-Mo3C
 with sigma of 0.04
 Cu1-Mo4B \\sim Cu1-Mo4C
 with sigma of 0.04
 C20B-Mo4B \\sim C20B-Mo4C
 with sigma of 0.04
 C19B-Mo4B \\sim C19B-Mo4C
 with sigma of 0.04
 C18B-Mo4B \\sim C18B-Mo4C
 with sigma of 0.04
 C17B-Mo4B \\sim C17B-Mo4C
 with sigma of 0.04
 C21B-Mo4B \\sim C21B-Mo4C
 with sigma of 0.04
 Mo3B-C22B \\sim Mo3C-C22B
 with sigma of 0.04
 Mo3B-Mo4B \\sim Mo3C-Mo4C
 with sigma of 0.04
 Mo3B-C25B \\sim Mo3C-C25B
 with sigma of 0.04
 Mo3B-C26B \\sim Mo3C-C26B
 with sigma of 0.04
 Mo3B-C27B \\sim Mo3C-C27B
 with sigma of 0.04
 Mo3B-C28B \\sim Mo3C-C28B
 with sigma of 0.04
 Mo3B-C24B \\sim Mo3C-C24B
 with sigma of 0.04
 Mo3B-Cu10 \\sim Mo3C-Cu10
 with sigma of 0.04
 C16B-Mo4B \\sim C16B-Mo4C
 with sigma of 0.04
 Mo4B-Cu10 \\sim Mo4C-Cu10
 with sigma of 0.04
 Mo4B-Cu11 \\sim Mo4C-Cu11
 with sigma of 0.04
 Cu11-Cu10 \\sim Cu2-Cu1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28B \\sim C28A \\sim C24B \\sim C24A \\sim C25A \\sim C25B \\sim C26A \\sim
C26B \\sim C27B \\sim C27A: within 1.9A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.9A
As2B \\sim Sb2A: within 2.9A with sigma of 0.001 and sigma for terminal atoms
of 0.01 within 2.9A
O7B \\sim O7A \\sim C22A \\sim C22B: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C22A \\sim C22B \\sim O7B \\sim O7A: within 1.9A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 1.9A
C17B \\sim C17A \\sim C18B \\sim C18A \\sim C19B \\sim C19A \\sim C20B \\sim
C20A \\sim C21B \\sim C21A: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
Mo3A \\sim Mo3B: within 1.9A with sigma of 0.01 and sigma for terminal atoms of
0.01 within 1.9A
Sb1A \\sim As1B \\sim Sb1B \\sim As1A: within 2.9A with sigma of 0.001 and
sigma for terminal atoms of 0.01 within 2.9A
C16B \\sim C16A \\sim O6A \\sim O6B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.01 within 1.7A
Mo3C \\sim Mo4B \\sim Mo4A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Mo3A \\sim Mo3B \\sim Mo4C: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
As2C \\sim As2A \\sim Sb2B \\sim Sb2C \\sim Sb2A \\sim As2B: within 3A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3A
Cu1 \\sim Cu10 \\sim Cu11 \\sim Cu2: within 3A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3A
As7 \\sim As1B \\sim Sb1A \\sim Sb2 \\sim Sb1B \\sim As1A: within 3A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 3A
Mo2 \\sim Mo4: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Mo3 \\sim Mo1: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(Mo3B) \\sim Ueq, Uanis(Mo3A) \\sim Ueq, Uanis(Mo4B) \\sim Ueq,
Uanis(Mo4A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Mo3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: Mo1(0.92) Mo2(0.92) Mo4A(0.59) As2B(0.33) Mo3A(0.59) As1A(0.46)
 Sb2B(0.33) Sb1A(0.46) Cu2(0.92) Cu1(0.92) O7A(0.52) C26A(0.52) H26A(0.52)
 C27A(0.52) H27A(0.52) C22A(0.52) C28A(0.52) H28A(0.52) O6A(0.58) N2A(0.56)
 C25A(0.52) H25A(0.52) C24A(0.52) H24A(0.52) C17A(0.58) H17A(0.58) C18A(0.58)
 H18A(0.58) C21A(0.58) H21A(0.58) C16A(0.58) C32A(0.56) H32A(0.56) H32B(0.56)
 H32C(0.56) As2A(0.59) Sb2A(0.59) Sb1B(0.46) As1B(0.46) C20A(0.58) H20A(0.58)
 C19A(0.58) H19A(0.58) C31A(0.56) C31B(0.44) N2B(0.44) C20B(0.42) H20B(0.42)
 C19B(0.42) H19B(0.42) C18B(0.42) H18B(0.42) C17B(0.42) H17B(0.42) C21B(0.42)
 H21B(0.42) Mo3B(0.33) C16B(0.42) O6B(0.42) Cl2A(0.58) Cl1A(0.58) Cl1B(0.42)
 Cl2B(0.42) C107(0.58) H10A(0.58) H10B(0.58) C108(0.42) H10C(0.42) H10D(0.42)
 C32B(0.44) H32D(0.44) H32E(0.44) H32F(0.44) C22B(0.48) O7B(0.48) Mo4B(0.33)
 C25B(0.48) H25B(0.48) C26B(0.48) H26B(0.48) C27B(0.48) H27B(0.48) C28B(0.48)
 H28B(0.48) C24B(0.48) H24B(0.48) Cu10(0.08) Cu11(0.08) Mo3C(0.08) Mo4C(0.08)
 As2C(0.08) Sb2C(0.08) Sb2(0.08) Mo3(0.08) Mo4(0.08) As7(0.08)
5.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C7(H7), C11(H11), C6(H6), C14(H14), C26A(H26A), C4(H4),
 C27A(H27A), C12(H12), C13(H13), C5(H5), C28A(H28A), C25A(H25A), C24A(H24A),
 C17A(H17A), C18A(H18A), C21A(H21A), C20A(H20A), C19A(H19A), C20B(H20B),
 C19B(H19B), C18B(H18B), C17B(H17B), C21B(H21B), C25B(H25B), C26B(H26B),
 C27B(H27B), C28B(H28B), C24B(H24B)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C32A(H32A,H32B,H32C), C32B(H32D,
 H32E,H32F)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 302 electrons were 
found in a volume of 1254\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1.8[CH2Cl2] per formula unit 
which account for 302 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38265
_shelx_hkl_checksum              61808
_shelx_fab_checksum              40182
_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
- B-factor correction
;