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_7132922
_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
'C56 H40 Ag2 As4 Mo8 O16 Sb4, 2(Al C36 F46 O3), C H2 Cl2'
_chemical_formula_sum            'C129 H42 Ag2 Al2 As4 Cl2 F92 Mo8 O22 Sb4'
_chemical_formula_weight         5586.42
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-26
_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                 91.7040(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.46640(10)
_cell_length_b                   40.5323(3)
_cell_length_c                   33.5837(2)
_cell_measurement_reflns_used    41228
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      71.5150
_cell_measurement_theta_min      4.0900
_cell_volume                     15601.4(2)
_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_temperature      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2548
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.971
_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    -38.00  43.00   0.50    7.50    --   39.90 -38.00  60.00  162
  2  \w    -43.00  27.00   0.50    7.50    --   39.90 -19.00   0.00  140
  3  \w    -20.00  81.00   0.50    7.50    --   39.90 -99.00 -30.00  202
  4  \w     24.00 105.00   0.50   25.00    --  105.16 -77.00 -90.00  162
  5  \w     39.00 130.00   0.50   25.00    --  105.16 178.00-150.00  182
  6  \w     20.00  80.00   0.50   25.00    --  105.16 -95.00 -90.00  120
  7  \w     80.00 178.00   0.50   25.00    --  105.16  77.00   0.00  196
  8  \w     20.00  80.00   0.50   25.00    --  105.16 -95.00   0.00  120
  9  \w     29.00  71.00   0.50   25.00    --  105.16 -61.00 -60.00   84
 10  \w     84.00 174.00   0.50   25.00    --  105.16  77.00  60.00  180
;
_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      -0.0162395000
_diffrn_orient_matrix_UB_12      0.0239463000
_diffrn_orient_matrix_UB_13      0.0349899000
_diffrn_orient_matrix_UB_21      -0.0765009000
_diffrn_orient_matrix_UB_22      -0.0257298000
_diffrn_orient_matrix_UB_23      0.0206780000
_diffrn_orient_matrix_UB_31      0.1093128000
_diffrn_orient_matrix_UB_32      -0.0144644000
_diffrn_orient_matrix_UB_33      0.0213152000
_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  0.0333
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            66428
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.725
_diffrn_reflns_theta_min         3.419
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.419
_exptl_absorpt_correction_T_max  0.233
_exptl_absorpt_correction_T_min  0.091
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.54a (Rigaku Oxford Diffraction, 2020)
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            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.378
_exptl_crystal_description       block
_exptl_crystal_F_000             10584
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.221
_exptl_crystal_size_min          0.181
_refine_diff_density_max         1.699
_refine_diff_density_min         -1.811
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2548
_refine_ls_number_reflns         29653
_refine_ls_number_restraints     164
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+22.3482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1137
_reflns_Friedel_coverage         0.000
_reflns_number_gt                27646
_reflns_number_total             29653
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01001a2.cif
_cod_data_source_block           psh_141_mp_abs_ana
_cod_depositor_comments
'Adding full bibliography for 7132918--7132923.cif.'
_cod_database_code               7132922
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C129H42Ag2Al2As4Cl2F92Mo8O22Sb4
_reflns_odcompleteness_completeness 99.28
_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
2. Restrained distances
 Sb4B-As4B \\sim Sb4A-As4A
 with sigma of 0.02
 Sb1B-As1B \\sim Sb1A-As1A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
As2A \\sim Sb2B \\sim Sb2A \\sim As2B: within 2.7A with sigma of 0.001 and
sigma for terminal atoms of 0.01 within 2.7A
As4A \\sim Sb4B \\sim Sb4A \\sim As4B: within 2.7A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2.7A
C7A \\sim C7B \\sim C6B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 1.7A
Sb3A \\sim As3A \\sim As3B \\sim Sb3B: within 2.7A with sigma of 0.001 and
sigma for terminal atoms of 0.01 within 2.7A
Ag2A \\sim Ag2B: within 2.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2.7A
As1A \\sim Sb1B \\sim As1B \\sim Sb1A: within 2.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 2.7A
4. Others
 Fixed Sof: Sb1A(0.8) Sb4A(0.86) Sb3A(0.72) Ag2A(0.62) Sb2A(0.65) As2A(0.65)
 As3A(0.72) As4A(0.86) As1A(0.8) Sb2B(0.35) As2B(0.35) As3B(0.28) Sb3B(0.28)
 O1A(0.53) C7A(0.53) H7A(0.53) C1A(0.53) C5A(0.53) H5A(0.53) C3A(0.53)
 H3A(0.53) C6A(0.53) H6A(0.53) C4A(0.53) H4A(0.53) C6B(0.47) H6B(0.47)
 C3B(0.47) H3B(0.47) C5B(0.47) H5B(0.47) C4B(0.47) H4B(0.47) O1B(0.47)
 O2A(0.53) C7B(0.47) H7B(0.47) C1B(0.47) C2B(0.47) O2B(0.47) C2A(0.53)
 As1B(0.2) Sb1B(0.2) Ag2B(0.38) As4B(0.14) Sb4B(0.14)
5.a Secondary CH2 refined with riding coordinates:
 C129(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C56(H56), C48(H48), C25(H25), C53(H53), C26(H26), C18(H18),
 C20(H20), C31(H31), C54(H54), C24(H24), C28(H28), C49(H49), C27(H27), C21(H21),
  C52(H52), C55(H55), C46(H46), C45(H45), C19(H19), C47(H47), C32(H32),
 C35(H35), C41(H41), C14(H14), C39(H39), C33(H33), C38(H38), C13(H13), C42(H42),
  C34(H34), C40(H40), C12(H12), C11(H11), C10(H10), C7A(H7A), C5A(H5A),
 C3A(H3A), C6A(H6A), C4A(H4A), C6B(H6B), C3B(H3B), C5B(H5B), C4B(H4B), C7B(H7B)
;
_shelx_res_checksum              19050
_shelx_hkl_checksum              83493
_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 1.904
_oxdiff_exptl_absorpt_empirical_full_min 0.602