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

data_7716434
_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         'C17 H21 As Mo O3 Si'
_chemical_formula_sum            'C17 H21 As Mo O3 Si'
_chemical_formula_weight         472.29
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_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            4
_cell_length_a                   6.65790(10)
_cell_length_b                   13.0043(2)
_cell_length_c                   22.3782(5)
_cell_measurement_reflns_used    3863
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6600
_cell_measurement_theta_min      5.1920
_cell_volume                     1937.53(6)
_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 0.999
_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    -96.00 -38.00   1.00    1.00    --  -37.08 -57.00  90.00   58
  2  \w     18.00  66.00   1.00    1.00    --   37.08  38.00 120.00   48
  3  \w    -28.00  37.00   1.00    1.00    --   37.08 -57.00 120.00   65
  4  \w     29.00  89.00   1.00    1.00    --   37.08-125.00 -30.00   60
  5  \w     43.00  70.00   1.00    1.00    --   37.08-125.00-120.00   27
  6  \w     46.00  71.00   1.00    1.00    --   37.08 -99.00  90.00   25
  7  \w     56.00  89.00   1.00    1.00    --  111.00 -50.00-180.00   33
  8  \w     57.00 105.00   1.00    1.00    --  111.00 -92.00 150.00   48
  9  \w    118.00 149.00   1.00    1.00    --  111.00  77.00-150.00   31
 10  \w     81.00 106.00   1.00    1.00    --  111.00 -92.00 -60.00   25
 11  \w     96.00 134.00   1.00    1.00    --  111.00  64.00 120.00   38
 12  \w     42.00  73.00   1.00    1.00    --  111.00-121.00-164.00   31
 13  \w     93.00 171.00   1.00    1.00    --  111.00  64.00-120.00   78
 14  \w     93.00 125.00   1.00    1.00    --  111.00 -50.00-180.00   32
 15  \w     94.00 119.00   1.00    1.00    --  111.00  25.00-150.00   25
 16  \w     72.00 100.00   1.00    1.00    --  111.00 -92.00-180.00   28
 17  \w    129.00 154.00   1.00    1.00    --  111.00  25.00-150.00   25
 18  \w     45.00  85.00   1.00    1.00    --  111.00 -50.00 150.00   40
 19  \w     73.00  98.00   1.00    1.00    --  111.00 -92.00-120.00   25
 20  \w    112.00 138.00   1.00    1.00    --  111.00  77.00   0.00   26
 21  \w     42.00  75.00   1.00    1.00    --  111.00 -92.00 120.00   33
;
_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      0.0419772000
_diffrn_orient_matrix_UB_12      -0.0652126000
_diffrn_orient_matrix_UB_13      0.0560921000
_diffrn_orient_matrix_UB_21      -0.0578514000
_diffrn_orient_matrix_UB_22      -0.0979891000
_diffrn_orient_matrix_UB_23      -0.0346396000
_diffrn_orient_matrix_UB_31      0.2200971000
_diffrn_orient_matrix_UB_32      -0.0134214000
_diffrn_orient_matrix_UB_33      -0.0197942000
_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  0.0269
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            7373
_diffrn_reflns_point_group_measured_fraction_full 0.945
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.817
_diffrn_reflns_theta_min         3.932
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.116
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.321
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       needle
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: pentane'
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.066
_refine_diff_density_max         0.396
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.335(14)
_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     214
_refine_ls_number_reflns         3665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0264
_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^)+(0.0271P)^2^+0.0582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0617
_reflns_Friedel_coverage         0.612
_reflns_Friedel_fraction_full    0.869
_reflns_Friedel_fraction_max     0.840
_reflns_number_gt                3515
_reflns_number_total             3665
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_219_b_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716434
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C17H21As1Mo1O3Si1
_chemical_oxdiff_usercomment     'hexane at -30'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.665(14)
 0.335(14)
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), C4(H4), C14(H14), C17(H17), C15(H15), C16(H16)
3.b Idealised Me refined as rotating group:
 C9(H9a,H9b,H9c), C10(H10a,H10b,H10c), C8(H8a,H8b,H8c), C12(H12a,H12b,H12c),
 C11(H11a,H11b,H11c)
;
_shelx_res_checksum              73362
_ins_header
;
TITL RMK_219_B_scale in P2(1)2(1)2(1) 
REM P2(1)2(1)2(1) (#19 in standard setting)
CELL 1.54184   6.657933  13.004326  22.378199  90.0000  90.0000  90.0000
ZERR    4.00   0.000123   0.000247   0.000467   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 Si As Mo
UNIT 68.00 84.00 12.00 4.00 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 1.275
_oxdiff_exptl_absorpt_empirical_full_min 0.778