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_7060284
_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         'C26 H19 Ag As3 Mo3 N O6, F6 P, C H2 Cl2'
_chemical_formula_sum            'C27 H21 Ag As3 Cl2 F6 Mo3 N O6 P'
_chemical_formula_weight         1291.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                90
_cell_angle_beta                 98.2656(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8486(4)
_cell_length_b                   18.8751(3)
_cell_length_c                   15.5925(3)
_cell_measurement_reflns_used    14488
_cell_measurement_temperature    123.11(10)
_cell_measurement_theta_max      74.2730
_cell_measurement_theta_min      3.9340
_cell_volume                     7237.2(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_environment      N~2~
_diffrn_ambient_temperature      123.11(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    -25.00  67.00   1.00    2.00    --   44.33 -57.00   0.00   92
  2  \w     35.00  91.00   1.00    6.00    --  104.50 -30.00 -30.00   56
  3  \w     44.00 135.00   1.00    6.00    --  104.50 -77.00 -30.00   91
  4  \w     78.00 120.00   1.00    6.00    --  104.50-125.00-120.00   42
  5  \w     34.00 123.00   1.00    2.00    --   44.33-178.00   0.00   89
  6  \w     38.00 130.00   1.00    6.00    --  104.50 -61.00  90.00   92
  7  \w     90.00 173.00   1.00    6.00    --  104.50  45.00 150.00   83
  8  \w     79.00 174.00   1.00    6.00    --  104.50  61.00-120.00   95
  9  \w     33.00  58.00   1.00    6.00    --  104.50-125.00-120.00   25
 10  \w     27.00 113.00   1.00    6.00    --  104.50-105.00 -63.00   86
 11  \w     32.00  88.00   1.00    6.00    --  104.50 -30.00-120.00   56
 12  \w   -116.00 -19.00   1.00    2.00    --  -44.33 -77.00 150.00   97
;
_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      0.0071370000
_diffrn_orient_matrix_UB_12      0.0279416000
_diffrn_orient_matrix_UB_13      0.0937965000
_diffrn_orient_matrix_UB_21      0.0430844000
_diffrn_orient_matrix_UB_22      0.0531012000
_diffrn_orient_matrix_UB_23      -0.0219758000
_diffrn_orient_matrix_UB_31      -0.0449214000
_diffrn_orient_matrix_UB_32      0.0553317000
_diffrn_orient_matrix_UB_33      -0.0261916000
_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  0.0305
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21960
_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         74.254
_diffrn_reflns_theta_min         2.951
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'GV50 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.091
_exptl_absorpt_correction_T_max  0.444
_exptl_absorpt_correction_T_min  0.144
_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    2.371
_exptl_crystal_description       block
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.179
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.868
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7156
_refine_ls_number_restraints     234
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0347P)^2^+13.2391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0650
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6547
_reflns_number_total             7156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj05959e2.cif
_cod_data_source_block           ems_404_mc_abs
_cod_depositor_comments
'Adding full bibliography for 7060280--7060285.cif.'
_cod_database_code               7060284
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C27H21AgAs3Cl2F6Mo3NO6P
_chemical_oxdiff_usercomment     'red block'
_shelx_estimated_absorpt_t_max   0.373
_shelx_estimated_absorpt_t_min   0.140
_reflns_odcompleteness_completeness 99.73
_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
2. Restrained distances
 Cl1B-C27B \\sim Cl2B-C27B
 with sigma of 0.02
 C21A-C20A \\sim C17A-C21A \\sim C20A-C19A
 with sigma of 0.02
 O5A-C15A \\sim O5B-C15B
 with sigma of 0.02
 O6A-C16A \\sim O6B-C16B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19A \\sim C18B \\sim C19B \\sim C20B \\sim C21A \\sim C20A \\sim C21B \\sim
C17A \\sim C17B: within 1.7A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 1.7A
O6A \\sim O6B \\sim C16B \\sim C16A \\sim C15B \\sim C15A \\sim O5A \\sim O5B:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 1.7A
Cl1B \\sim C27B \\sim Cl2B \\sim Cl2A \\sim C27A: within 1.9A with sigma of
0.02 and sigma for terminal atoms of 0.02 within 1.9A
Uanis(C27B) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: As3A(0.5) O5A(0.5) C15A(0.5) O6A(0.5) C16A(0.5) Cl1A(0.65)
 Cl2A(0.65) C27A(0.65) H27A(0.65) H27B(0.65) Cl2B(0.35) Cl1B(0.35) C27B(0.35)
 H27C(0.35) H27D(0.35) As3B(0.5) O6B(0.5) C16B(0.5) C15B(0.5) O5B(0.5)
 C17A(0.5) H17A(0.5) C21A(0.5) H21A(0.5) C20A(0.5) H20A(0.5) C19A(0.5)
 H19A(0.5) C20B(0.5) H20B(0.5) C19B(0.5) H19B(0.5) C18B(0.5) H18B(0.5)
 H17B(0.5) H17C(0.5) C21B(0.5) H21B(0.5)
5.a Ternary CH refined with riding coordinates:
 C17B(H17B), C17B(H17C)
5.b Secondary CH2 refined with riding coordinates:
 C27A(H27A,H27B), C27B(H27C,H27D)
5.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C3(H3), C10(H10), C4(H4), C12(H12), C11(H11), C14(H14), C5(H5),
 C6(H6), C25(H25), C7(H7), C22(H22), C26(H26), C23(H23), C17A(H17A), C21A(H21A),
  C20A(H20A), C19A(H19A), C20B(H20B), C19B(H19B), C18B(H18B), C21B(H21B)
;
_shelx_res_checksum              69479
_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 3.223
_oxdiff_exptl_absorpt_empirical_full_min 0.745