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_7132918
_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         '2(C28 H20 As2 Cl2 Cu2 Mo4 O8 Sb2)'
_chemical_formula_sum            'C56 H40 As4 Cl4 Cu4 Mo8 O16 Sb4'
_chemical_formula_weight         2919.04
_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             2018-03-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.03.09 svn.r3491 for OlexSys, GUI svn.r5480)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                89.358(3)
_cell_angle_beta                 89.116(3)
_cell_angle_gamma                69.160(4)
_cell_formula_units_Z            2
_cell_length_a                   15.0550(6)
_cell_length_b                   15.1827(9)
_cell_length_c                   17.1422(4)
_cell_measurement_reflns_used    7884
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      31.6580
_cell_measurement_theta_min      4.9790
_cell_volume                     3661.4(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      123(1)
_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 0.896
_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    -93.00  11.00   0.25  120.00    --  -18.71 -57.00-180.00  416
  2  \w    -97.00  15.00   0.25  120.00    --  -18.71 -77.00  60.00  448
  3  \w   -100.00  28.00   0.25  120.00    --  -18.71 -19.00-120.00  512
  4  \w     53.00 108.00   0.25  120.00    --   19.49-178.00 -30.00  220
  5  \w     57.00  70.00   0.25  120.00    --   19.49 178.00-150.00   52
;
_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      -0.0058051000
_diffrn_orient_matrix_UB_12      0.0141637000
_diffrn_orient_matrix_UB_13      -0.0397485000
_diffrn_orient_matrix_UB_21      -0.0055725000
_diffrn_orient_matrix_UB_22      -0.0430133000
_diffrn_orient_matrix_UB_23      -0.0097128000
_diffrn_orient_matrix_UB_31      -0.0497822000
_diffrn_orient_matrix_UB_32      0.0211790000
_diffrn_orient_matrix_UB_33      0.0062359000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_unetI/netI     0.0052
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26111
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.486
_diffrn_reflns_theta_min         3.114
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.898
_exptl_absorpt_correction_T_max  0.710
_exptl_absorpt_correction_T_min  0.631
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.648
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.087
_refine_diff_density_max         2.730
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.262
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         26111
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.259
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0184P)^2^+143.1096P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25134
_reflns_number_total             26111
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9307\% 
 around [0.71 0.71 -0.00] (reciprocal) or [0.72 0.70 -0.02] (direct)
;
_cod_data_source_file            d4cc01001a2.cif
_cod_data_source_block           test2abs_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7132918--7132923.cif.'
_cod_database_code               7132918
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C56H40As4Cl4Cu4Mo8O16Sb
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.514
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.7764(11)
 0.2236(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Uiso/Uaniso restraints and constraints
As3A \\sim Sb3B \\sim Sb3A \\sim As3B: within 2.8A with sigma of 0.001 and
sigma for terminal atoms of 0.001
As2B \\sim Sb2A \\sim As2A \\sim Sb2B: within 2.8A with sigma of 0.001 and
sigma for terminal atoms of 0.001
Sb1A \\sim As1B \\sim As1A \\sim Sb1B: within 2.8A with sigma of 0.001 and
sigma for terminal atoms of 0.001
As4A \\sim Sb4B \\sim Sb4A \\sim As4B: within 2.8A with sigma of 0.001 and
sigma for terminal atoms of 0.001
4. Others
 Sof(Sb1B)=Sof(As1B)=1-FVAR(1)
 Sof(As1A)=Sof(Sb1A)=FVAR(1)
 Sof(Sb2B)=Sof(As2B)=1-FVAR(2)
 Sof(As2A)=Sof(Sb2A)=FVAR(2)
 Sof(As3B)=Sof(Sb3B)=1-FVAR(3)
 Sof(Sb3A)=Sof(As3A)=FVAR(3)
 Sof(Sb4B)=Sof(As4B)=1-FVAR(4)
 Sof(As4A)=Sof(Sb4A)=FVAR(4)
5.a Aromatic/amide H refined with riding coordinates:
 C18(H18), C10(H10), C53(H53), C32(H32), C19(H19), C35(H35), C48(H48),
 C54(H54), C28(H28), C7(H7), C3(H3), C39(H39), C52(H52), C11(H11), C42(H42),
 C33(H33), C55(H55), C27(H27), C49(H49), C21(H21), C24(H24), C20(H20), C12(H12),
  C14(H14), C4(H4), C38(H38), C31(H31), C40(H40), C5(H5), C13(H13), C45(H45),
 C34(H34), C26(H26), C56(H56), C17(H17), C41(H41), C6(H6), C46(H46), C47(H47),
 C25(H25)
;
_shelx_res_checksum              24745
_shelx_hkl_checksum              63688
_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 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.764
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2