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_7060281
_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
'C21 H17 Ag As2 Mo2 N2 O4, C2 H3 N, F6 P1, 1.5[C2H3N]'
_chemical_formula_sum            'C23 H20 Ag As2 F6 Mo2 N3 O4 P'
_chemical_formula_weight         996.98
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-03-16
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-12-03 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                100.5570(10)
_cell_angle_beta                 111.5570(10)
_cell_angle_gamma                100.6310(10)
_cell_formula_units_Z            2
_cell_length_a                   10.8770(2)
_cell_length_b                   13.3926(2)
_cell_length_c                   13.6762(2)
_cell_measurement_reflns_used    12332
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      69.6790
_cell_measurement_theta_min      3.2180
_cell_volume                     1751.08(5)
_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 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_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    -22.00  28.00   0.50    4.50    --  -43.14  38.00 150.00  100
  2  \w    -27.00  69.00   0.50    4.50    --   43.14 -57.00-120.00  192
  3  \w     18.00 113.00   0.50    4.50    --   43.14  57.00  30.00  190
  4  \w     97.00 170.00   0.50   17.50    --   95.79 125.00 120.00  146
  5  \w     26.00  93.00   0.50   17.50    --   95.79 -61.00 -90.00  134
  6  \w     27.00 112.00   0.50   17.50    --   95.79-125.00 120.00  170
  7  \w     17.00  46.00   0.50   17.50    --   95.79 -15.00 -30.00   58
  8  \w     13.00 106.00   0.50   17.50    --   95.79 -95.00-120.00  186
  9  \w     23.00  57.00   0.50   17.50    --   95.79 -30.00   0.00   68
 10  \w     17.00  46.00   0.50   17.50    --   95.79 -15.00  90.00   58
 11  \w     23.00  57.00   0.50   17.50    --   95.79 -30.00 120.00   68
 12  \w     71.00 166.00   0.50   17.50    --   95.79  45.00 -90.00  190
 13  \w     22.00 127.00   0.50   17.50    --   95.79 -77.00 120.00  210
 14  \w     18.00 113.00   0.50    4.50    --   43.14  57.00-180.00  190
 15  \w     18.00 113.00   0.50    4.50    --   43.14  57.00 120.00  190
 16  \w     18.00 113.00   0.50    4.50    --   43.14  57.00 -90.00  190
 17  \w     69.00 169.00   0.50   17.50    --   95.79  30.00 150.00  200
 18  \w     71.00 166.00   0.50   17.50    --   95.79  45.00  60.00  190
;
_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      -0.0281904000
_diffrn_orient_matrix_UB_12      -0.1094013000
_diffrn_orient_matrix_UB_13      -0.0346162000
_diffrn_orient_matrix_UB_21      0.0510410000
_diffrn_orient_matrix_UB_22      -0.0034169000
_diffrn_orient_matrix_UB_23      0.1084213000
_diffrn_orient_matrix_UB_31      -0.1307457000
_diffrn_orient_matrix_UB_32      -0.0109137000
_diffrn_orient_matrix_UB_33      -0.0019671000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\b'
_diffrn_radiation_wavelength     1.39222
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21688
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        56.650
_diffrn_reflns_theta_max         69.506
_diffrn_reflns_theta_min         3.153
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.962
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.363
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_description       block
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.062
_refine_diff_density_max         1.020
_refine_diff_density_min         -1.200
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         8567
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0327P)^2^+0.7930P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0718
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7586
_reflns_number_total             8567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05959e2.cif
_cod_data_source_block           js233_ap_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7060280--7060285.cif.'
_cod_original_cell_volume        1751.07(5)
_cod_database_code               7060281
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AgAs2C26F6H24.5Mo2N4.5O4P
_shelx_estimated_absorpt_t_max   0.577
_shelx_estimated_absorpt_t_min   0.307
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     63.18
_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. Restrained distances
 P1B-F6B \\sim P1B-F2B \\sim P1B-F3B \\sim P1B-F5B \\sim P1B-F4B \\sim P1C-F4C
\\sim P1A-F6A \\sim P1C-F1C
 \\sim P1A-F4A \\sim P1A-F5A \\sim P1A-F1A \\sim P1C-F2C \\sim P1C-F5C \\sim
P1A-F2A \\sim P1B-F1B \\sim P1C-
 F3C \\sim P1A-F3A \\sim P1C-F6C
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F3B, P1B, F6B, F2B, F1B, F5B, F4B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3C, P1C, F1C, F2C, F4C, F5C, F6C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F3A, P1A, F4A, F5A, F2A, F6A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: Mo2A(0.58) Mo1A(0.76) O4A(0.58) C14A(0.58) C18A(0.63) H18A(0.63)
 C19A(0.63) H19A(0.63) C4A(0.68) H4A(0.68) C12A(0.58) H12A(0.58) O1A(0.68)
 O3B(0.58) C3A(0.68) H3A(0.68) C8A(0.58) H8A(0.58) C5A(0.68) H5A(0.68)
 C9A(0.58) H9A(0.58) O2A(0.68) C1A(0.68) H1A(0.68) C13B(0.58) C2A(0.68)
 H2A(0.68) C7A(0.68) C6A(0.68) C11A(0.58) H11A(0.58) C10A(0.58) H10A(0.58)
 C11B(0.42) H11B(0.42) C10B(0.42) H10B(0.42) C9B(0.42) H9B(0.42) C8B(0.42)
 H8B(0.42) C12B(0.42) H12B(0.42) C14B(0.42) O4B(0.42) O3A(0.42) C13A(0.42)
 C6B(0.32) O1B(0.32) C3B(0.32) H3B(0.32) C4B(0.32) H4B(0.32) C5B(0.32)
 H5B(0.32) C1B(0.32) H1B(0.32) C2B(0.32) H2B(0.32) O2B(0.32) C7B(0.32)
 C18B(0.37) H18B(0.37) C19B(0.37) H19B(0.37) Mo1B(0.24) Mo2B(0.42) P1A(0.35)
 F4A(0.35) F5A(0.35) F2A(0.35) F6A(0.35) F1A(0.35) F3A(0.35) P1B(0.25)
 F4B(0.25) F1B(0.25) F2B(0.25) F3B(0.25) F6B(0.25) F5B(0.25) P1C(0.4) F1C(0.4)
 F2C(0.4) F3C(0.4) F4C(0.4) F5C(0.4) F6C(0.4)
5.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C16(H16), C18A(H18A), C19A(H19A), C4A(H4A), C12A(H12A), C3A(H3A),
 C8A(H8A), C5A(H5A), C9A(H9A), C1A(H1A), C2A(H2A), C11A(H11A), C10A(H10A),
 C11B(H11B), C10B(H10B), C9B(H9B), C8B(H8B), C12B(H12B), C3B(H3B), C4B(H4B),
 C5B(H5B), C1B(H1B), C2B(H2B), C18B(H18B), C19B(H19B)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95613
_shelx_fab_checksum              54275
_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 1.928
_oxdiff_exptl_absorpt_empirical_full_min 0.594