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_7132919
_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         'C14 H10 As Cu I Mo2 O4 Sb, C H2 Cl2'
_chemical_formula_sum            'C15 H12 As Cl2 Cu I Mo2 O4 Sb'
_chemical_formula_weight         906.14
_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             2018-03-13
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.03.09 svn.r3491 for OlexSys, GUI svn.r5479)
;
_audit_update_record
;
2024-02-01 deposited with the CCDC.	2024-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.374(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4347(4)
_cell_length_b                   15.6404(6)
_cell_length_c                   13.4725(4)
_cell_measurement_reflns_used    5897
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      31.7210
_cell_measurement_theta_min      3.7610
_cell_volume                     2196.86(14)
_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)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.883
_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    -65.00  61.00   0.50   90.00    --  -18.71  19.00  60.00  252
  2  \w     58.00  99.00   0.50   90.00    --   19.65 178.00 150.00   82
  3  \w     57.00 110.00   0.50   90.00    --   19.65 178.00 -90.00  106
;
_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      0.0237456000
_diffrn_orient_matrix_UB_12      -0.0215507000
_diffrn_orient_matrix_UB_13      -0.0417827000
_diffrn_orient_matrix_UB_21      -0.0467221000
_diffrn_orient_matrix_UB_22      -0.0324920000
_diffrn_orient_matrix_UB_23      0.0051298000
_diffrn_orient_matrix_UB_31      -0.0435382000
_diffrn_orient_matrix_UB_32      0.0230683000
_diffrn_orient_matrix_UB_33      -0.0316529000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0472
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13681
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.472
_diffrn_reflns_theta_min         3.256
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.448
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.434
_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    2.740
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.043
_refine_diff_density_max         1.672
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         7011
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0479
_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^)+(0.0326P)^2^+1.4293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5969
_reflns_number_total             7011
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01001a2.cif
_cod_data_source_block           ems_635_mp_abs
_cod_depositor_comments
'Adding full bibliography for 7132918--7132923.cif.'
_cod_database_code               7132919
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C15H12AsCl2CuIMo2O4Sb
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1A-C15A \\sim Cl2A-C15A \\sim Cl2B-C15B \\sim Cl1B-C15B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl1B \\sim Cl1A \\sim C15A \\sim C15B \\sim Cl2A \\sim Cl2B: within 1.8A with
sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(Cl2B)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(Cl1B)=1-FVAR(1)
 Sof(Cl1A)=Sof(Cl2A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=FVAR(1)
 Sof(As1B)=Sof(Sb1B)=1-FVAR(2)
 Sof(Sb1A)=Sof(As1A)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C15A(H15A,H15B), C15B(H15C,H15D)
5.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C10(H10), C13(H13), C7(H7), C4(H4), C14(H14), C3(H3),
 C5(H5), C6(H6)
;
_shelx_res_checksum              56948
_shelx_hkl_checksum              64455
_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 1.932
_oxdiff_exptl_absorpt_empirical_full_min 0.719