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_7060280
_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
'C68 H50 Ag2 As8 Mo8 N2 O16, 2(F6 P), 2(C2 H3 N), 2.7(C H2 Cl2)'
_chemical_formula_sum            'C74.7 H61.4 Ag2 As8 Cl5.4 F12 Mo8 N4 O16 P2'
_chemical_formula_weight         3335.06
_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             2020-01-13
_audit_creation_method
;
Olex2 1.3-alpha
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-12-03 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                97.822(2)
_cell_angle_beta                 103.366(3)
_cell_angle_gamma                91.281(2)
_cell_formula_units_Z            1
_cell_length_a                   12.9052(4)
_cell_length_b                   12.9624(3)
_cell_length_c                   16.0579(5)
_cell_measurement_reflns_used    19466
_cell_measurement_temperature    122.97(13)
_cell_measurement_theta_max      74.4660
_cell_measurement_theta_min      3.3970
_cell_volume                     2585.09(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14a (Rigaku OD, 2018)'
_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      122.97(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.958
_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   1.00    1.00    --   44.08  57.00   0.00   93
  2  \w    -25.00  68.00   1.00    1.00    --   44.08 -57.00-150.00   93
  3  \w     34.00 130.00   1.00    1.00    --   44.08-178.00-180.00   96
  4  \w     36.00  98.00   1.00    1.00    --  104.50 -45.00  30.00   62
  5  \w     33.00 135.00   1.00    1.00    --  104.50 -77.00 -60.00  102
  6  \w     32.00  91.00   1.00    1.00    --  104.50 -30.00  90.00   59
  7  \w     33.00 121.00   1.00    1.00    --  104.50-125.00-180.00   88
  8  \w     82.00 173.00   1.00    1.00    --  104.50  45.00-150.00   91
  9  \w     32.00  91.00   1.00    1.00    --  104.50 -30.00 -60.00   59
 10  \w     33.00 135.00   1.00    1.00    --  104.50 -77.00-180.00  102
 11  \w     27.00 141.00   1.00    1.00    --  104.50 -15.00-180.00  114
 12  \w     14.00 116.00   1.00    1.00    --   44.08  77.00 150.00  102
 13  \w     20.00 113.00   1.00    1.00    --   44.08  57.00  90.00   93
 14  \w     20.00 113.00   1.00    1.00    --   44.08  57.00 -90.00   93
 15  \w     82.00 173.00   1.00    1.00    --  104.50  45.00 -90.00   91
 16  \w     81.00 177.00   1.00    1.00    --  104.50  30.00   0.00   96
;
_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      0.0989354000
_diffrn_orient_matrix_UB_12      -0.0651159000
_diffrn_orient_matrix_UB_13      0.0188639000
_diffrn_orient_matrix_UB_21      -0.0728954000
_diffrn_orient_matrix_UB_22      -0.0996091000
_diffrn_orient_matrix_UB_23      -0.0136724000
_diffrn_orient_matrix_UB_31      -0.0003450000
_diffrn_orient_matrix_UB_32      -0.0165694000
_diffrn_orient_matrix_UB_33      -0.0969045000
_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  0.0347
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24671
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.232
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    15.754
_exptl_absorpt_correction_T_max  0.263
_exptl_absorpt_correction_T_min  0.029
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14a (Rigaku Oxford Diffraction, 2018)
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    2.142
_exptl_crystal_description       block
_exptl_crystal_F_000             1589
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.209
_refine_diff_density_max         1.132
_refine_diff_density_min         -1.386
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       0.00124(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         10080
_refine_ls_number_restraints     130
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0611P)^2^+2.5543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9574
_reflns_number_total             10080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05959e2.cif
_cod_data_source_block           ems_405_ap_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7060280--7060285.cif.'
_cod_original_formula_sum
'C74.70 H61.40 Ag2 As8 Cl5.40 F12 Mo8 N4 O16 P2'
_cod_database_code               7060280
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C76H64Ag2As8Cl8F12Mo8N4O16P2
_chemical_oxdiff_usercomment     'red block'
_shelx_estimated_absorpt_t_max   0.137
_shelx_estimated_absorpt_t_min   0.078
_reflns_odcompleteness_completeness 99.26
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.29
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl2-C37 = Cl1-C37
 1.77 with sigma of 0.01
 Cl5-Cl6
 2.9 with sigma of 0.02
 Cl1-C37 \\sim Cl2-C37
 with sigma of 0.02
 Cl3-C1A \\sim Cl4-C1A \\sim Cl5-C1B \\sim Cl6-C1B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C37 \\sim Cl2 \\sim Cl1: within 1.9A with sigma of 0.02 and sigma for terminal
atoms of 0.04 within 1.9A
C1B \\sim Cl3 \\sim C1A \\sim Cl4 \\sim Cl5 \\sim Cl6: within 1.9A with sigma
of 0.02 and sigma for terminal atoms of 0.04 within 1.9A
F5B \\sim F5A \\sim F2B \\sim F3B \\sim F1B \\sim F3A \\sim P1: within 1.9A
with sigma of 0.2 and sigma for terminal atoms of 0.2 within 1.9A
4. Others
 Fixed Sof: F3A(0.65) F5A(0.65) F6A(0.65) F4A(0.65) F1A(0.65) F2A(0.65)
 F5B(0.35) F1B(0.35) F4B(0.35) F6B(0.35) F2B(0.35) F3B(0.35) Cl1(0.75)
 Cl2(0.75) C37(0.75) H37A(0.75) H37B(0.75) Cl3(0.4) Cl4(0.4) C1A(0.4) H1AA(0.4)
 H1AB(0.4) Cl5(0.2) Cl6(0.2) C1B(0.2) H1BA(0.2) H1BB(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C1A(H1AA,H1AB), C1B(H1BA,H1BB)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C30(H30), C29(H29), C32(H32), C12(H12), C33(H33), C14(H14),
 C13(H13), C7(H7), C11(H11), C6(H6), C34(H34), C20(H20), C19(H19), C24(H24),
 C5(H5), C17(H17), C25(H25), C10(H10), C21(H21), C18(H18), C26(H26), C28(H28),
 C27(H27)
5.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C)
;
_shelx_res_checksum              85880
_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 1.883
_oxdiff_exptl_absorpt_empirical_full_min 0.723