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_7060283
_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         'C22 H16 Ag As2 Mo2 N4 O4, F6 P'
_chemical_formula_sum            'C22 H16 Ag As2 F6 Mo2 N4 O4 P'
_chemical_formula_weight         994.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-10-18
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2020-12-03 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.817(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5558(3)
_cell_length_b                   21.4306(5)
_cell_length_c                   10.6865(2)
_cell_measurement_reflns_used    10790
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      74.3010
_cell_measurement_theta_min      3.5350
_cell_volume                     2814.56(11)
_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 (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_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.969
_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     20.00 113.00   0.75    3.00    --   44.08  57.00 -90.00  124
  2  \w     21.00 114.00   0.75    3.00    --   44.08  38.00   0.00  124
  3  \w     23.00 108.50   0.75    9.00    --  104.50 -94.00 -60.00  114
  4  \w     82.00 172.00   0.75    9.00    --  104.50  45.00-180.00  120
  5  \w     23.00 108.50   0.75    9.00    --  104.50 -94.00   0.00  114
  6  \w     36.00  97.50   0.75    9.00    --  104.50 -45.00  60.00   82
  7  \w     36.00  97.50   0.75    9.00    --  104.50 -45.00   0.00   82
  8  \w    -50.00  26.50   0.75    3.00    --  -44.08  38.00 -90.00  102
  9  \w     20.00 113.00   0.75    3.00    --   44.08  57.00 120.00  124
 10  \w     79.00 173.50   0.75    9.00    --  104.50  61.00   0.00  126
 11  \w     68.00  98.00   0.75    9.00    --  104.50  15.00 120.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV 50, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0225458000
_diffrn_orient_matrix_UB_12      -0.0040423000
_diffrn_orient_matrix_UB_13      -0.1470208000
_diffrn_orient_matrix_UB_21      0.1176978000
_diffrn_orient_matrix_UB_22      0.0207909000
_diffrn_orient_matrix_UB_23      0.0012084000
_diffrn_orient_matrix_UB_31      0.0368690000
_diffrn_orient_matrix_UB_32      -0.0686745000
_diffrn_orient_matrix_UB_33      0.0090366000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15640
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.231
_diffrn_reflns_theta_min         3.596
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.591
_exptl_absorpt_correction_T_max  0.387
_exptl_absorpt_correction_T_min  0.152
_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    2.348
_exptl_crystal_description       block
_exptl_crystal_F_000             1896
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.104
_refine_diff_density_max         2.640
_refine_diff_density_min         -1.871
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0590
_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^)+(0.1198P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5096
_reflns_number_total             5559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05959e2.cif
_cod_data_source_block           ems_542f_mp_abs
_cod_depositor_comments
'Adding full bibliography for 7060280--7060285.cif.'
_cod_database_code               7060283
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C22H16AgAs2F6Mo2N4O4P
_chemical_oxdiff_usercomment     'orange blocks'
_shelx_estimated_absorpt_t_max   0.277
_shelx_estimated_absorpt_t_min   0.134
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C20(H20), C5(H5), C4(H4), C17(H17), C6(H6), C15(H15),
 C13(H13), C7(H7), C3(H3), C16(H16), C11(H11), C14(H14), C10(H10), C12(H12)
;
_shelx_res_checksum              63369
_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
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 5.690
_oxdiff_exptl_absorpt_empirical_full_min 0.139