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_7132921
_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
'C30 H23 As2 Cu Mo4 N O8 Sb2, Al C36 F46 O3, C H2 Cl2'
_chemical_formula_sum            'C67 H25 Al As2 Cl2 Cu F46 Mo4 N O11 Sb2'
_chemical_formula_weight         2832.40
_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             2020-06-17
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.05.22 svn.r1d9e7f8d for OlexSys, GUI svn.r6115)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.2370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.9582(2)
_cell_length_b                   33.3030(4)
_cell_length_c                   12.1289(2)
_cell_measurement_reflns_used    23996
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.8670
_cell_measurement_theta_min      3.8700
_cell_volume                     8168.03(19)
_computing_cell_refinement       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.54a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.54a (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_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.950
_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     -5.00  31.00   1.00    1.00    --  -44.92  19.00 -60.00   36
  2  \w     -5.00  31.00   1.00    1.00    --  -44.92  19.00  90.00   36
  3  \w     -5.00  31.00   1.00    1.00    --  -44.92  19.00   0.00   36
  4  \w     -5.00  31.00   1.00    1.00    --  -44.92  19.00 -30.00   36
  5  \w     27.00  98.00   1.00    1.00    --   44.92-125.00-180.00   71
  6  \w     35.00  93.00   1.00    4.00    --  104.50 -61.00 120.00   58
  7  \w     35.00  93.00   1.00    4.00    --  104.50 -61.00  60.00   58
  8  \w    103.00 176.00   1.00    4.00    --  104.50  77.00-180.00   73
  9  \w     36.00  72.00   1.00    4.00    --  104.50 -45.00 150.00   36
 10  \w     30.00 178.00   1.00    4.00    --  104.50   0.00   0.00  148
 11  \w   -113.00 -88.00   1.00    1.00    --  -44.92 -57.00   0.00   25
 12  \w   -113.00 -21.00   1.00    1.00    --  -44.92 -57.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0466891000
_diffrn_orient_matrix_UB_12      0.0324406000
_diffrn_orient_matrix_UB_13      -0.0672883000
_diffrn_orient_matrix_UB_21      -0.0590250000
_diffrn_orient_matrix_UB_22      -0.0287958000
_diffrn_orient_matrix_UB_23      -0.0131975000
_diffrn_orient_matrix_UB_31      -0.0114902000
_diffrn_orient_matrix_UB_32      0.0160867000
_diffrn_orient_matrix_UB_33      0.1124445000
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            36804
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.061
_diffrn_reflns_theta_min         3.438
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.448
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.012
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (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    2.303
_exptl_crystal_description       block
_exptl_crystal_F_000             5392
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.265
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.158
_refine_ls_extinction_coef       0.000046(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1302
_refine_ls_number_reflns         15774
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0743P)^2^+17.2915P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1231
_refine_ls_wR_factor_ref         0.1255
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14735
_reflns_number_total             15774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01001a2.cif
_cod_data_source_block           psh_133_mp_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7132918--7132923.cif.'
_cod_database_code               7132921
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C67H23AlAs2Cl2CuF46Mo4NO11Sb2
_shelx_estimated_absorpt_t_max   0.377
_shelx_estimated_absorpt_t_min   0.035
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 Sb1B-As1B \\sim Sb1A-As1A
 with sigma of 0.02
 Cl1A-C67A \\sim Cl2A-C67A \\sim Cl1B-C67B \\sim Cl2B-C67B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
As1A \\sim Sb1B \\sim As1B \\sim Sb1A: within 2.8A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2.8A
C67B \\sim Cl2B \\sim C67A \\sim Cl1A \\sim Cl2A \\sim Cl1B: within 1.9A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.9A
4. Others
 Sof(As1B)=Sof(Sb1B)=1-FVAR(1)
 Sof(Sb1A)=Sof(As1A)=FVAR(1)
 Sof(Sb2B)=Sof(As2B)=1-FVAR(2)
 Sof(Sb2A)=Sof(As2A)=FVAR(2)
 Sof(Cl2B)=Sof(Cl1B)=Sof(C67B)=Sof(H67C)=Sof(H67D)=1-FVAR(3)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C67A)=Sof(H67A)=Sof(H67B)=FVAR(3)
5.a Secondary CH2 refined with riding coordinates:
 C67A(H67A,H67B), C67B(H67C,H67D)
5.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C26(H26), C7(H7), C21(H21), C17(H17), C24(H24), C27(H27), C13(H13),
 C14(H14), C6(H6), C3(H3), C5(H5), C28(H28), C20(H20), C12(H12), C10(H10),
 C4(H4), C11(H11), C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C)
;
_shelx_res_checksum              97206
_shelx_hkl_checksum              68616
_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 1.719
_oxdiff_exptl_absorpt_empirical_full_min 0.688