σ-Arsolido complexes.
Kirk, Ryan M.; HIll, Anthony F; Dalton transactions (Cambridge, England : 2003) 53 (2024) 11809–11829; doi:10.1039/d4dt01308e

data_7716435
_publ_section_title
;
 &#x3c3;-Arsolido complexes.
;
_journal_issue                   28
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11809
_journal_page_last               11829
_journal_paper_doi               10.1039/d4dt01308e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C16 H17 As Mo O3'
_chemical_formula_sum            'C16 H17 As Mo O3'
_chemical_formula_weight         428.15
_chemical_properties_physical    Air-sensitive
_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             2022-01-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-01-29 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                78.829(3)
_cell_angle_beta                 88.971(3)
_cell_angle_gamma                72.297(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6134(2)
_cell_length_b                   7.7893(2)
_cell_length_c                   14.8554(6)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.9290
_cell_measurement_theta_min      6.0660
_cell_volume                     822.56(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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    -62.00  32.00   1.00    2.00    --  -36.63  19.00 -30.00   94
  2  \w    -55.00  33.00   1.00    2.00    --  -36.63  38.00-150.00   88
  3  \w    -53.00  31.00   1.00    2.00    --  -36.63  38.00 120.00   84
  4  \w    -54.00 -12.00   1.00    2.00    --  -36.63 125.00 -51.00   42
  5  \w     24.00  58.00   1.00    2.00    --   36.63  57.00  90.00   34
  6  \w      7.00 104.00   1.00    2.00    --   36.63  19.00-120.00   97
  7  \w     14.00  51.00   1.00    2.00    --   36.63  70.00 124.52   37
  8  \w     19.00  62.00   1.00    2.00    --   36.63  38.00-180.00   43
  9  \w     24.00  99.00   1.00    2.00    --   36.63  64.00 -41.73   75
 10  \w     28.00  57.00   1.00    2.00    --   36.63 -77.00-180.00   29
 11  \w     65.00  91.00   1.00    2.00    --   36.63  73.00-112.13   26
 12  \w     21.00  46.00   1.00    2.00    --   36.63  57.00 -60.00   25
 13  \w     21.00  47.00   1.00    2.00    --   36.63  57.00  60.00   26
 14  \w     20.00  87.00   1.00    2.00    --   36.63  38.00  90.00   67
 15  \w     20.00  46.00   1.00    2.00    --   36.63  57.00  30.00   26
 16  \w     69.00  94.00   1.00    2.00    --   36.63  57.00  90.00   25
 17  \w     14.00  53.00   1.00    2.00    --   36.63  73.00-112.13   39
 18  \w     40.00  72.00   1.00    2.00    --   36.63-125.00 -30.00   32
 19  \w     13.00  62.00   1.00    2.00    --   36.63  72.00-168.61   49
 20  \w     51.00  87.00   1.00    2.00    --   36.63-125.00 120.00   36
 21  \w     92.00 133.00   1.00    5.00    --  109.00  61.00  60.00   41
 22  \w     41.00 126.00   1.00    5.00    --  109.00 -45.00-180.00   85
 23  \w     40.00  67.00   1.00    5.00    --  109.00-111.00 -60.00   27
 24  \w     92.00 118.00   1.00    5.00    --  109.00  45.00-150.00   26
 25  \w    139.00 166.00   1.00    5.00    --  109.00  61.00  90.00   27
 26  \w    153.00 178.00   1.00    5.00    --  109.00  30.00-180.00   25
 27  \w    124.00 149.00   1.00    5.00    --  109.00  45.00-150.00   25
 28  \w     55.00  81.00   1.00    5.00    --  109.00 -95.00-180.00   26
 29  \w     93.00 139.00   1.00    5.00    --  109.00  45.00 -90.00   46
 30  \w    139.00 165.00   1.00    5.00    --  109.00  61.00  60.00   26
 31  \w     91.00 117.00   1.00    5.00    --  109.00  61.00  90.00   26
 32  \w    124.00 151.00   1.00    5.00    --  109.00  45.00 150.00   27
 33  \w     92.00 117.00   1.00    5.00    --  109.00  45.00 150.00   25
 34  \w     93.00 152.00   1.00    5.00    --  109.00  45.00  30.00   59
 35  \w     90.00 115.00   1.00    5.00    --  109.00  30.00-180.00   25
 36  \w     44.00  73.00   1.00    5.00    --  109.00 -77.00-180.00   29
 37  \w     93.00 123.00   1.00    5.00    --  109.00  45.00 120.00   30
 38  \w     92.00 156.00   1.00    5.00    --  109.00  45.00 -30.00   64
 39  \w    137.00 175.00   1.00    5.00    --  109.00  61.00-150.00   38
 40  \w     92.00 117.00   1.00    5.00    --  109.00  61.00-150.00   25
 41  \w    148.00 173.00   1.00    5.00    --  109.00  61.00 120.00   25
 42  \w    151.00 176.00   1.00    5.00    --  109.00  61.00 -30.00   25
 43  \w    132.00 169.00   1.00    5.00    --  109.00 111.00   0.00   37
 44  \w    125.00 164.00   1.00    5.00    --  109.00  45.00 120.00   39
 45  \w     91.00 117.00   1.00    5.00    --  109.00  61.00 -30.00   26
 46  \w     85.00 111.00   1.00    5.00    --  109.00 -77.00-180.00   26
 47  \w     91.00 118.00   1.00    5.00    --  109.00  61.00 120.00   27
 48  \w     94.00 144.00   1.00    5.00    --  109.00  45.00   0.00   50
 49  \w     93.00 120.00   1.00    5.00    --  109.00  45.00  60.00   27
 50  \w     92.00 117.00   1.00    5.00    --  109.00  61.00   0.00   25
 51  \w    133.00 158.00   1.00    5.00    --  109.00  61.00   0.00   25
 52  \w     92.00 117.00   1.00    5.00    --  109.00  61.00-180.00   25
 53  \w    134.00 176.00   1.00    5.00    --  109.00  61.00-180.00   42
 54  \w     93.00 134.00   1.00    5.00    --  109.00  45.00  90.00   41
 55  \w    138.00 164.00   1.00    5.00    --  109.00  45.00 -60.00   26
 56  \w     91.00 166.00   1.00    5.00    --  109.00  61.00  30.00   75
 57  \w     40.00  73.00   1.00    5.00    --  109.00-111.00-180.00   33
 58  \w     84.00 109.00   1.00    5.00    --  109.00-111.00-180.00   25
 59  \w     84.00 109.00   1.00    5.00    --  109.00-111.00  90.00   25
 60  \w     92.00 123.00   1.00    5.00    --  109.00  61.00 -60.00   31
 61  \w     93.00 125.00   1.00    5.00    --  109.00  45.00 -60.00   32
 62  \w     91.00 173.00   1.00    5.00    --  109.00  61.00 -90.00   82
 63  \w     93.00 119.00   1.00    5.00    --  109.00  45.00-180.00   26
 64  \w     41.00  75.00   1.00    5.00    --  109.00-111.00  90.00   34
 65  \w     43.00  94.00   1.00    5.00    --  109.00 -61.00 -60.00   51
 66  \w     89.00 115.00   1.00    5.00    --  109.00  30.00 120.00   26
 67  \w     92.00 129.00   1.00    5.00    --  109.00  30.00  30.00   37
 68  \w     92.00 124.00   1.00    5.00    --  109.00  30.00-120.00   32
 69  \w     92.00 118.00   1.00    5.00    --  109.00  61.00-120.00   26
 70  \w     58.00 106.00   1.00    5.00    --  109.00 -95.00-150.00   48
 71  \w     39.00  86.00   1.00    5.00    --  109.00 -30.00 120.00   47
 72  \w     46.00  72.00   1.00    5.00    --  109.00-111.00  60.00   26
 73  \w     73.00 109.00   1.00    5.00    --  109.00-111.00  60.00   36
 74  \w     39.00 107.00   1.00    5.00    --  109.00-111.00 150.00   68
 75  \w     91.00 152.00   1.00    5.00    --  109.00  30.00 -30.00   61
 76  \w     77.00 102.00   1.00    5.00    --  109.00  15.00-120.00   25
 77  \w     88.00 115.00   1.00    5.00    --  109.00  30.00   0.00   27
 78  \w     45.00  90.00   1.00    5.00    --  109.00-111.00   0.00   45
 79  \w     47.00  97.00   1.00    5.00    --  109.00-111.00  30.00   50
 80  \w    141.00 171.00   1.00    5.00    --  109.00  45.00-120.00   30
 81  \w     91.00 118.00   1.00    5.00    --  109.00  61.00 150.00   27
 82  \w    143.00 173.00   1.00    5.00    --  109.00  61.00 150.00   30
 83  \w     46.00  78.00   1.00    5.00    --  109.00-111.00 120.00   32
 84  \w     84.00 109.00   1.00    5.00    --  109.00-111.00 120.00   25
 85  \w    112.00 139.00   1.00    5.00    --  109.00 111.00  60.00   27
 86  \w    148.00 173.00   1.00    5.00    --  109.00 111.00  60.00   25
 87  \w     92.00 118.00   1.00    5.00    --  109.00  45.00-120.00   26
 88  \w     89.00 122.00   1.00    5.00    --  109.00  30.00 -90.00   33
 89  \w     76.00 107.00   1.00    5.00    --  109.00-111.00 -60.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.2107083000
_diffrn_orient_matrix_UB_12      -0.0383228000
_diffrn_orient_matrix_UB_13      -0.0017596000
_diffrn_orient_matrix_UB_21      -0.0107632000
_diffrn_orient_matrix_UB_22      0.0266768000
_diffrn_orient_matrix_UB_23      -0.1054680000
_diffrn_orient_matrix_UB_31      -0.0263318000
_diffrn_orient_matrix_UB_32      0.2065858000
_diffrn_orient_matrix_UB_33      -0.0081263000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0183
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9139
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.152
_diffrn_reflns_theta_min         6.079
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.814
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-pentane'
_exptl_crystal_size_max          0.193
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         9139
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0779P)^2^+0.6294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8625
_reflns_number_total             9139
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9961\% 
around [0.00 -0.00 1.00] (reciprocal) or [0.08 -0.37 0.93] (direct)
;
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_219_a_scale_twin_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716435
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C16 H17 As1 Mo1 O3 '
_chemical_oxdiff_usercomment     'pentane evap at -30'
_shelx_estimated_absorpt_t_max   0.488
_shelx_estimated_absorpt_t_min   0.281
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6737(10)
 0.3263(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C12(H12), C14(H14), C15(H15)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              55712
_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 1.225
_oxdiff_exptl_absorpt_empirical_full_min 0.852
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2