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_7060285
_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         'C90 H80 Ag4 As8 Mo8 N8 O16, 4(F6 P)'
_chemical_formula_sum            'C90 H80 Ag4 As8 F24 Mo8 N8 O16 P4'
_chemical_formula_weight         3907.86
_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             2020-01-31
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2020.01.31 svn.r88ba2a32 for OlexSys, GUI svn.r6020)
;
_audit_update_record
;
2020-12-03 deposited with the CCDC.	2021-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                79.429(2)
_cell_angle_beta                 87.128(2)
_cell_angle_gamma                77.470(2)
_cell_formula_units_Z            2
_cell_length_a                   10.7861(2)
_cell_length_b                   20.7482(4)
_cell_length_c                   26.5944(5)
_cell_measurement_reflns_used    34095
_cell_measurement_temperature    122.97(12)
_cell_measurement_theta_max      74.0760
_cell_measurement_theta_min      4.1610
_cell_volume                     5710.9(2)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.97(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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     -5.00  31.00   1.00    1.17    --  -44.92  19.00-180.00   36
  2  \w     -5.00  31.00   1.00    1.17    --  -44.92  19.00  30.00   36
  3  \w   -119.00  29.00   1.00    1.17    --  -44.92   0.00-180.00  148
  4  \w     15.00  42.00   1.00    1.17    --   44.92  76.00-158.33   27
  5  \w     27.00  98.00   1.00    1.17    --   44.92-125.00  90.00   71
  6  \w     23.00 106.00   1.00    4.68    --  104.50 -94.00 -90.00   83
  7  \w     82.00 173.00   1.00    4.68    --  104.50  44.00 164.41   91
  8  \w     50.00  72.00   1.00    4.68    --  104.50 -45.00-180.00   22
  9  \w     81.00 177.00   1.00    4.68    --  104.50  30.00  60.00   96
 10  \w    103.00 176.00   1.00    4.68    --  104.50  77.00  90.00   73
 11  \w     33.00 127.00   1.00    4.68    --  104.50 -77.00  60.00   94
 12  \w     36.00  72.00   1.00    4.68    --  104.50 -45.00  60.00   36
 13  \w     28.00 108.00   1.00    4.68    --  104.50-108.00  28.68   80
 14  \w     33.00 120.00   1.00    4.68    --  104.50-135.00-102.60   87
 15  \w     14.00  42.00   1.00    1.17    --   44.92  79.00 -90.41   28
 16  \w     14.00  42.00   1.00    1.17    --   44.92  79.00 151.86   28
 17  \w     15.00  42.00   1.00    1.17    --   44.92  77.00 113.48   27
 18  \w     21.00 113.00   1.00    1.17    --   44.92  57.00  30.00   92
 19  \w     78.00 173.00   1.00    4.68    --  104.50  66.00-147.88   95
 20  \w     77.00 174.00   1.00    4.68    --  104.50  69.00 101.21   97
 21  \w     68.00 178.00   1.00    4.68    --  104.50  15.00 -30.00  110
 22  \w     79.00 117.00   1.00    4.68    --  104.50  61.00-180.00   38
 23  \w     77.00 173.00   1.00    4.68    --  104.50  67.00 -18.31   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      -0.0492400000
_diffrn_orient_matrix_UB_12      -0.0487672000
_diffrn_orient_matrix_UB_13      0.0432400000
_diffrn_orient_matrix_UB_21      -0.1356653000
_diffrn_orient_matrix_UB_22      0.0257235000
_diffrn_orient_matrix_UB_23      -0.0210589000
_diffrn_orient_matrix_UB_31      0.0240888000
_diffrn_orient_matrix_UB_32      -0.0541540000
_diffrn_orient_matrix_UB_33      -0.0340550000
_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  0.0468
_diffrn_reflns_av_unetI/netI     0.0469
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            63285
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.148
_diffrn_reflns_theta_min         3.381
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.312
_exptl_absorpt_correction_T_max  0.411
_exptl_absorpt_correction_T_min  0.182
_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    2.273
_exptl_crystal_description       block
_exptl_crystal_F_000             3736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1463
_refine_ls_number_reflns         22500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20378
_reflns_number_total             22500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05959e2.cif
_cod_data_source_block           js2016_ap_abs_gaus
_cod_depositor_comments
'Adding full bibliography for 7060280--7060285.cif.'
_cod_database_code               7060285
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C90H80Ag4As8F24Mo8N8O16P4
_shelx_estimated_absorpt_t_max   0.267
_shelx_estimated_absorpt_t_min   0.193
_reflns_odcompleteness_completeness 99.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Secondary CH2 refined with riding coordinates:
 C68(H68A,H68B), C24(H24A,H24B), C67(H67A,H67B), C69(H69A,H69B), C22(H22A,
 H22B), C23(H23A,H23B)
2.b Aromatic/amide H refined with riding coordinates:
 C57(H57), C71(H71), C18(H18), C56(H56), C21(H21), C73(H73), C70(H70),
 C44(H44), C10(H10), C14(H14), C20(H20), C65(H65), C48(H48), C66(H66), C74(H74),
  C81(H81), C28(H28), C63(H63), C26(H26), C17(H17), C29(H29), C82(H82),
 C86(H86), C52(H52), C3(H3), C43(H43), C45(H45), C62(H62), C59(H59), C58(H58),
 C49(H49), C7(H7), C11(H11), C12(H12), C50(H50), C13(H13), C5(H5), C35(H35),
 C41(H41), C80(H80), C90(H90), C51(H51), C42(H42), C25(H25), C55(H55), C4(H4),
 C36(H36), C6(H6), C79(H79), C34(H34), C87(H87), C89(H89), C88(H88), C38(H38),
 C37(H37), C83(H83)
2.c Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C31(H31A,H31B,H31C), C16(H16A,H16B,H16C), C76(H76A,H76B,
 H76C)
;
_shelx_res_checksum              13673
_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 1.384
_oxdiff_exptl_absorpt_empirical_full_min 0.804