Discrete and polymeric organometallic-organic assemblies based on the diarsene complex [(Cp)2Mo2(CO)4(μ,η2-As2)], AgPF6 and N-donor organic molecules
Moussa, Mehdi Elsayed; Schiller, Jana; Seidl, Michael; Shelyganov, Pavel A.; Scheer, Manfred; New Journal of Chemistry 45 (2021) 1800–1804; doi:10.1039/D0NJ05959E

data_7060282
_publ_section_title
;
 Discrete and polymeric organometallic-organic assemblies based on the
 diarsene complex [(Cp)2Mo2(CO)4(\m,\h2-As2)], AgPF6 and N-donor organic
 molecules
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1800
_journal_page_last               1804
_journal_paper_doi               10.1039/D0NJ05959E
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety
'C34 H24 Ag As4 Mo4 N O8, F6 P, C2 H3 N, 1.5[CH2Cl2]'
_chemical_formula_sum            'C37.5 H30 Ag As4 Cl3 F6 Mo4 N2 O8 P'
_chemical_formula_weight         1679.26
_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             2020-11-27
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6197)
;
_audit_update_record
;
2020-12-03 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                98.621(4)
_cell_angle_beta                 103.144(4)
_cell_angle_gamma                90.062(4)
_cell_formula_units_Z            2
_cell_length_a                   12.8682(7)
_cell_length_b                   13.0664(6)
_cell_length_c                   15.9420(8)
_cell_measurement_reflns_used    12390
_cell_measurement_temperature    123.0(2)
_cell_measurement_theta_max      74.2030
_cell_measurement_theta_min      2.8390
_cell_volume                     2579.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41h (Rigaku OD, 2015)'
_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      123.0(2)
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.936
_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    -25.00  68.00   1.00    1.00    --   44.45 -57.00-150.00   93
  2  \w     35.00 126.00   1.00    2.00    --  104.50 -77.00 -60.00   91
  3  \w     81.00 177.00   1.00    2.00    --  104.50  30.00 -90.00   96
  4  \w    143.00 169.00   1.00    2.00    --  104.50  77.00  60.00   26
  5  \w     83.00 116.00   1.00    2.00    --  104.50  77.00  60.00   33
  6  \w     81.00 177.00   1.00    2.00    --  104.50  30.00   0.00   96
  7  \w     43.00 121.00   1.00    2.00    --  104.50-125.00 150.00   78
  8  \w     39.00 135.00   1.00    2.00    --  104.50 -77.00 150.00   96
  9  \w     32.00  91.00   1.00    2.00    --  104.50 -30.00  90.00   59
 10  \w     32.00  90.00   1.00    2.00    --  104.50 -30.00 -30.00   58
 11  \w     36.00 127.00   1.00    1.00    --   44.45 178.00-150.00   91
 12  \w   -114.00 -19.00   1.00    1.00    --  -44.45 -75.00  -8.00   95
;
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16266
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.868
_diffrn_reflns_theta_min         2.881
_exptl_absorpt_coefficient_mu    15.937
_exptl_absorpt_correction_T_max  0.274
_exptl_absorpt_correction_T_min  0.046
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41h (Rigaku Oxford Diffraction, 2015)
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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.162
_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.907
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         9905
_refine_ls_number_restraints     150
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0605P)^2^+2.2554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9308
_reflns_number_total             9905
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05959e2.cif
_cod_data_source_block           ems_407_ap_abs
_cod_depositor_comments
'Adding full bibliography for 7060280--7060285.cif.'
_cod_original_formula_sum        'C37.50 H30 Ag As4 Cl3 F6 Mo4 N2 O8 P'
_cod_database_code               7060282
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.193
_shelx_estimated_absorpt_t_min   0.072
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
F3B \\sim P1 \\sim F4A \\sim F6A \\sim F5A \\sim F2A \\sim F1A \\sim F3A \\sim
F1B \\sim F4B \\sim F6B \\sim F2B \\sim F5B: within 1.9A with sigma of 0.01 and
sigma for terminal atoms of 0.01 within 1.9A
3. Others
 Sof(F1B)=Sof(F4B)=Sof(F6B)=Sof(F2B)=Sof(F3B)=Sof(F5B)=1-FVAR(1)
 Sof(F4A)=Sof(F6A)=Sof(F5A)=Sof(F2A)=Sof(F1A)=Sof(F3A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C9(H9), C10(H10), C17(H17), C29(H29), C15(H15), C30(H30), C21(H21),
 C11(H11), C13(H13), C32(H32), C25(H25), C18(H18), C12(H12), C26(H26), C33(H33),
  C22(H22), C28(H28), C20(H20), C24(H24), C23(H23), C27(H27), C14(H14), C19(H19)
4.b Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 138 electrons were 
found in a volume of 490\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.5[CH2Cl2] per Asymmetric Unit 
which account for 126 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9210
_shelx_fab_checksum              78021
_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
;