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

data_7716441
_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 H24 As2 Cl2'
_chemical_formula_sum            'C16 H24 As2 Cl2'
_chemical_formula_weight         437.09
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 141.48(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.355(4)
_cell_length_b                   9.7741(6)
_cell_length_c                   20.102(5)
_cell_measurement_reflns_used    3885
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      31.6660
_cell_measurement_theta_min      3.7020
_cell_volume                     1757(2)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1872
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.880
_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    -38.00  14.00   1.00    7.50    --  -17.69 -77.00  30.00   52
  2  \w     -7.00  32.00   1.00    7.50    --   18.00  77.00 -60.00   39
  3  \w     40.00  91.00   1.00    7.50    --   18.00  37.00  90.00   51
  4  \w    -42.00  50.00   1.00    7.50    --   18.00 -77.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0082980000
_diffrn_orient_matrix_UB_12      -0.0619437000
_diffrn_orient_matrix_UB_13      -0.0133756000
_diffrn_orient_matrix_UB_21      -0.0423352000
_diffrn_orient_matrix_UB_22      0.0279511000
_diffrn_orient_matrix_UB_23      -0.0502236000
_diffrn_orient_matrix_UB_31      0.0665846000
_diffrn_orient_matrix_UB_32      0.0254625000
_diffrn_orient_matrix_UB_33      0.0225594000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12271
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.401
_diffrn_reflns_theta_min         3.254
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.653
_exptl_crystal_description       prism
_exptl_crystal_F_000             880
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.222
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         5547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0377
_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^)+(0.0292P)^2^+0.1706P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0811
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4275
_reflns_number_total             5547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_222_b_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_original_cell_volume        1756.7(14)
_cod_database_code               7716441
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C16H24As2Cl2
_shelx_estimated_absorpt_t_max   0.463
_shelx_estimated_absorpt_t_min   0.312
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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:
 C12(H12a,H12b,H12c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C16(H16a,H16b,
 H16c), C10(H10a,H10b,H10c), C13(H13a,H13b,H13c), C15(H15a,H15b,H15c), C14(H14a,
 H14b,H14c)
;
_ins_header
;
TITL RMK_222_B_scale in P2(1)/n 
REM P2(1)/n (#14 in standard setting)
CELL 0.71073  14.354757   9.774118  20.101855  90.0000 141.4760  90.0000
ZERR    4.00   0.003632   0.000621   0.005020   0.0000   0.0528   0.0000
LATT  1
SYMM -x+1/2, y+1/2,-z+1/2 
SFAC C H Cl As
UNIT 64.00 96.00 8.00 8.00
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 1.093
_oxdiff_exptl_absorpt_empirical_full_min 0.910