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

data_7716437
_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         'C14 H24 As Cl'
_chemical_formula_sum            'C14 H24 As Cl'
_chemical_formula_weight         302.70
_chemical_properties_physical    Air-sensitive,Moisture-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             2022-01-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-05-31 deposited with the CCDC.	2024-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                80.871(3)
_cell_angle_beta                 81.879(3)
_cell_angle_gamma                77.842(3)
_cell_formula_units_Z            4
_cell_length_a                   9.0412(3)
_cell_length_b                   11.8621(4)
_cell_length_c                   14.5361(5)
_cell_measurement_reflns_used    8295
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.1150
_cell_measurement_theta_min      4.6080
_cell_volume                     1495.27(9)
_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 2018/2 (Sheldrick, 2018)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_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    -99.00 -56.00   1.00    1.00    --  -36.63 -57.00 -60.00   43
  2  \w    -75.00  -7.00   1.00    1.00    --  -36.63 125.00 -90.00   68
  3  \w    -53.00  30.00   1.00    1.00    --  -36.63  57.00 -90.00   83
  4  \w   -105.00 -19.00   1.00    1.00    --  -36.63 -38.00 120.00   86
  5  \w    -92.00 -18.00   1.00    1.00    --  -36.63 -38.00  30.00   74
  6  \w     51.00  89.00   1.00    1.00    --   36.63-125.00-150.00   38
  7  \w     46.00  76.00   1.00    1.00    --   36.63 -99.00  30.00   30
  8  \w     39.00  65.00   1.00    1.00    --   36.63-125.00-180.00   26
  9  \w     43.00 104.00   1.00    1.00    --   36.63  57.00  30.00   61
 10  \w     53.00 109.00   1.00    1.00    --  109.00 -45.00 -90.00   56
 11  \w     67.00 109.00   1.00    1.00    --  109.00-111.00 120.00   42
 12  \w    111.00 137.00   1.00    1.00    --  109.00 178.00-150.00   26
 13  \w    115.00 141.00   1.00    1.00    --  109.00 -15.00 -60.00   26
 14  \w     83.00 127.00   1.00    1.00    --  109.00 -30.00-180.00   44
 15  \w    133.00 176.00   1.00    1.00    --  109.00  15.00-180.00   43
 16  \w    107.00 134.00   1.00    1.00    --  109.00 -80.00 140.48   27
 17  \w     80.00 129.00   1.00    1.00    --  109.00 -30.00  90.00   49
 18  \w     94.00 134.00   1.00    1.00    --  109.00 -77.00-120.00   40
 19  \w     81.00 130.00   1.00    1.00    --  109.00 -30.00 -60.00   49
 20  \w     39.00  75.00   1.00    1.00    --  109.00 -30.00  90.00   36
 21  \w     72.00 108.00   1.00    1.00    --  109.00-111.00  30.00   36
 22  \w     71.00 121.00   1.00    1.00    --  109.00  15.00-180.00   50
 23  \w     50.00  76.00   1.00    1.00    --  109.00 -45.00-150.00   26
 24  \w     43.00  73.00   1.00    1.00    --  109.00 -95.00-120.00   30
 25  \w     77.00 104.00   1.00    1.00    --  109.00 -95.00-120.00   27
 26  \w     40.00  90.00   1.00    1.00    --  109.00 -15.00 -60.00   50
 27  \w     42.00  67.00   1.00    1.00    --  109.00 -95.00 -60.00   25
 28  \w     39.00  67.00   1.00    1.00    --  109.00 -30.00-180.00   28
 29  \w     40.00  66.00   1.00    1.00    --  109.00 -30.00 -60.00   26
 30  \w     44.00  86.00   1.00    1.00    --  109.00 -45.00  60.00   42
 31  \w     52.00  78.00   1.00    1.00    --  109.00 -95.00-150.00   26
 32  \w     94.00 127.00   1.00    1.00    --  109.00 -77.00   0.00   33
 33  \w     42.00 109.00   1.00    1.00    --  109.00-111.00 -30.00   67
 34  \w     68.00 108.00   1.00    1.00    --  109.00-111.00  60.00   40
 35  \w     52.00 120.00   1.00    1.00    --  109.00 -45.00 -30.00   68
 36  \w     50.00  76.00   1.00    1.00    --  109.00-111.00-120.00   26
 37  \w     84.00 109.00   1.00    1.00    --  109.00-111.00-120.00   25
 38  \w     76.00 126.00   1.00    1.00    --  109.00 -61.00  90.00   50
 39  \w    119.00 152.00   1.00    1.00    --  109.00  30.00 -60.00   33
 40  \w     66.00  92.00   1.00    1.00    --  109.00 -77.00-120.00   26
 41  \w     91.00 124.00   1.00    1.00    --  109.00 -45.00  60.00   33
 42  \w    141.00 166.00   1.00    1.00    --  109.00  61.00-120.00   25
 43  \w     73.00 106.00   1.00    1.00    --  109.00 -95.00 120.00   33
 44  \w     79.00 107.00   1.00    1.00    --  109.00-111.00-150.00   28
 45  \w     44.00  69.00   1.00    1.00    --  109.00-111.00 -90.00   25
 46  \w    120.00 145.00   1.00    1.00    --  109.00 111.00 120.00   25
 47  \w     97.00 155.00   1.00    1.00    --  109.00  15.00-120.00   58
 48  \w     94.00 136.00   1.00    1.00    --  109.00 -20.00-162.34   42
 49  \w    134.00 161.00   1.00    1.00    --  109.00   0.00-180.00   27
 50  \w     40.00  82.00   1.00    1.00    --  109.00 -20.00-162.34   42
;
_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      -0.0095061000
_diffrn_orient_matrix_UB_12      -0.0681008000
_diffrn_orient_matrix_UB_13      -0.0801451000
_diffrn_orient_matrix_UB_21      -0.1701754000
_diffrn_orient_matrix_UB_22      0.0551012000
_diffrn_orient_matrix_UB_23      -0.0007075000
_diffrn_orient_matrix_UB_31      0.0414189000
_diffrn_orient_matrix_UB_32      0.1014620000
_diffrn_orient_matrix_UB_33      -0.0724161000
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15607
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.248
_diffrn_reflns_theta_min         3.846
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.495
_exptl_absorpt_correction_T_max  0.61961
_exptl_absorpt_correction_T_min  0.58982
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_description       needle
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.071
_exptl_crystal_size_rad          0.079
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         5973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+0.3132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5407
_reflns_number_total             5973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_230_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716437
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C14H24As1Cl1
_chemical_oxdiff_usercomment     'hexane evap'
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C12(H12A,H12B,H12C),
 C28(H28A,H28B,H28C), C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C20(H20A,H20B,
 H20C), C9(H9A,H9B,H9C), C27(H27A,H27B,H27C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C23(H23A,H23B,H23C), C11(H11A,H11B,H11C), C26(H26A,H26B,H26C),
 C10(H10A,H10B,H10C)
;
_shelx_res_checksum              37979
_ins_header
;
TITL RMK_230_scale in P-1 
REM P-1 (#2 in standard setting)
CELL 1.54184   9.041228  11.862147  14.536115  80.8715  81.8789  77.8419
ZERR    4.00   0.000294   0.000351   0.000488   0.0026   0.0027   0.0026
LATT  1
SFAC C H Cl As
UNIT 56.00 96.00 4.00 4.00
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 1.799
_oxdiff_exptl_absorpt_empirical_full_min 0.730