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

data_7716440
_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         'C36 H25 As Mo O3, C6 H6'
_chemical_formula_sum            'C42 H31 As Mo O3'
_chemical_formula_weight         754.53
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.87950(10)
_cell_length_b                   15.39100(10)
_cell_length_c                   23.5717(2)
_cell_measurement_reflns_used    23102
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.5580
_cell_measurement_theta_min      4.4140
_cell_volume                     6849.33(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1297
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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    -44.00 -11.00   1.00    5.00    --  -36.95  57.00-180.00   33
  2  \w    -34.00  -6.00   1.00    5.00    --  -36.95 125.00-150.00   28
  3  \w     29.00  90.00   1.00    5.00    --   36.95-125.00 120.00   61
  4  \w    -24.00  49.00   1.00    5.00    --   36.95 -38.00   0.00   73
  5  \w     28.00  90.00   1.00    5.00    --   36.95-125.00 -60.00   62
  6  \w     45.00  74.00   1.00    5.00    --   36.95-125.00  60.00   29
  7  \w     14.00  58.00   1.00    5.00    --   36.95 -99.00 -60.00   44
  8  \w      8.00  76.00   1.00    5.00    --   36.95 -99.00 -30.00   68
  9  \w     41.00  66.00   1.00    5.00    --   36.95 -99.00  60.00   25
 10  \w     54.00  92.00   1.00   30.00    --  111.00 -92.00 -60.00   38
 11  \w    139.00 178.00   1.00   30.00    --  111.00  76.00 -24.00   39
 12  \w     44.00 108.00   1.00   30.00    --  111.00 -38.00 -60.00   64
 13  \w     78.00 103.00   1.00   30.00    --  111.00-111.00  90.00   25
 14  \w    122.00 147.00   1.00   30.00    --  111.00  64.00  60.00   25
 15  \w     79.00 105.00   1.00   30.00    --  111.00 -92.00-180.00   26
 16  \w     64.00 107.00   1.00   30.00    --  111.00-111.00 -60.00   43
 17  \w    142.00 172.00   1.00   30.00    --  111.00  64.00-180.00   30
 18  \w     95.00 121.00   1.00   30.00    --  111.00  64.00-180.00   26
 19  \w     45.00  98.00   1.00   30.00    --  111.00 -92.00  90.00   53
 20  \w     43.00 101.00   1.00   30.00    --  111.00 -92.00-150.00   58
 21  \w     56.00 108.00   1.00   30.00    --  111.00-111.00  30.00   52
 22  \w    106.00 155.00   1.00   30.00    --  111.00  77.00  30.00   49
 23  \w     64.00  96.00   1.00   30.00    --  111.00 -92.00  30.00   32
 24  \w     68.00  94.00   1.00   30.00    --  111.00 -92.00 150.00   26
 25  \w    104.00 135.00   1.00   30.00    --  111.00 111.00   0.00   31
 26  \w     68.00 129.00   1.00   30.00    --  111.00 -38.00-180.00   61
 27  \w    130.00 159.00   1.00   30.00    --  111.00  77.00-120.00   29
 28  \w     44.00 107.00   1.00   30.00    --  111.00 -50.00  90.00   63
 29  \w    104.00 153.00   1.00   30.00    --  111.00 111.00 120.00   49
 30  \w    106.00 131.00   1.00   30.00    --  111.00 111.00  90.00   25
 31  \w     50.00  75.00   1.00   30.00    --  111.00-111.00  60.00   25
 32  \w     60.00 101.00   1.00   30.00    --  111.00 -64.00 -90.00   41
 33  \w     90.00 116.00   1.00   30.00    --  111.00 -64.00  30.00   26
 34  \w     70.00  95.00   1.00   30.00    --  111.00 -92.00 -30.00   25
 35  \w     73.00  98.00   1.00   30.00    --  111.00 -92.00 120.00   25
 36  \w    150.00 167.00   1.00   30.00    --  111.00  77.00  60.00   17
;
_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      0.0483788000
_diffrn_orient_matrix_UB_12      -0.0036127000
_diffrn_orient_matrix_UB_13      0.0525395000
_diffrn_orient_matrix_UB_21      0.0380449000
_diffrn_orient_matrix_UB_22      0.0830967000
_diffrn_orient_matrix_UB_23      -0.0200297000
_diffrn_orient_matrix_UB_31      -0.0535769000
_diffrn_orient_matrix_UB_32      0.0558299000
_diffrn_orient_matrix_UB_33      0.0332137000
_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  0.0241
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            45669
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.893
_diffrn_reflns_theta_min         3.750
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.508
_exptl_absorpt_correction_T_max  0.66605
_exptl_absorpt_correction_T_min  0.64271
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    1.463
_exptl_crystal_description       prism
_exptl_crystal_F_000             3056
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/n-hexane'
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.062
_exptl_crystal_size_rad          0.053
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         6909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0427P)^2^+4.3693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0746
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6265
_reflns_number_total             6909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_158_b_2_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716440
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C36H30As1Mo1O3
_chemical_oxdiff_usercomment     'benzene/hexane at -20'
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C14(H14), C26(H26), C32(H32), C36(H36), C30(H30), C29(H29), C15(H15),
 C33(H33), C4(H4), C18(H18), C35(H35), C34(H34), C20(H20), C28(H28), C24(H24),
 C16(H16), C5(H5), C27(H27), C39(H39), C8(H8), C17(H17), C38(H38), C6(H6),
 C40(H40), C42(H42), C37(H37), C7(H7), C22(H22), C41(H41), C21(H21), C23(H23)
;
_shelx_res_checksum              48802
_ins_header
;
TITL RMK_158_B_2_scale in Pbca 
REM Pbca (#61, found as Pcab in ba-c setting)
CELL 1.54184  18.879474  15.390970  23.571728  90.0000  90.0000  90.0000
ZERR    9.00   0.000142   0.000119   0.000167   0.0000   0.0000   0.0000
LATT  1
SYMM -x+1/2,-y, z+1/2 
SYMM -x, y+1/2,-z+1/2 
SYMM  x+1/2,-y+1/2,-z 
SFAC C H O As Mo
UNIT 324.00 270.00 27.00 9.00 9.00
TREF
HKLF 4
END
;
_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 1.518
_oxdiff_exptl_absorpt_empirical_full_min 0.816