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

data_7716439
_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         'C28 H20 As, C7 H5 Fe O2'
_chemical_formula_sum            'C35 H25 As Fe O2'
_chemical_formula_weight         608.32
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 91.4300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.34180(10)
_cell_length_b                   15.50870(10)
_cell_length_c                   17.76510(10)
_cell_measurement_reflns_used    20980
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.6090
_cell_measurement_theta_min      4.9550
_cell_volume                     5602.70(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 0.996
_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   -101.00  13.00   1.00    1.50    --  -36.95   0.00   0.00  114
  2  \w     29.00  58.00   1.00    1.50    --   36.95-125.00  90.00   29
  3  \w     51.00  90.00   1.00    1.50    --   36.95-125.00   0.00   39
  4  \w    -12.00  61.00   1.00    1.50    --   36.95 -19.00-150.00   73
  5  \w     42.00  90.00   1.00    1.50    --   36.95  57.00 -30.00   48
  6  \w     63.00 103.00   1.00    1.50    --   36.95  57.00   0.00   40
  7  \w     -6.00  47.00   1.00    1.50    --   36.95 -57.00 150.00   53
  8  \w     51.00  78.00   1.00    1.50    --   36.95-125.00 120.00   27
  9  \w     42.00 102.00   1.00    1.50    --   36.95  57.00-150.00   60
 10  \w     29.00  89.00   1.00    1.50    --   36.95-125.00 -60.00   60
 11  \w     20.00 106.00   1.00    1.50    --   36.95  38.00-180.00   86
 12  \w     60.00  86.00   1.00    1.50    --   36.95  57.00  30.00   26
 13  \w     23.00  82.00   1.00    1.50    --   36.95-120.00 137.00   59
 14  \w     42.00 102.00   1.00    7.50    --  111.00-111.00   0.00   60
 15  \w    135.00 160.00   1.00    7.50    --  111.00 111.00 -90.00   25
 16  \w     66.00  92.00   1.00    7.50    --  111.00 -92.00 150.00   26
 17  \w     62.00 105.00   1.00    7.50    --  111.00 -92.00-180.00   43
 18  \w     45.00  95.00   1.00    7.50    --  111.00-111.00 150.00   50
 19  \w     98.00 151.00   1.00    7.50    --  111.00  38.00 -90.00   53
 20  \w     80.00 123.00   1.00    7.50    --  111.00 -50.00-150.00   43
 21  \w     80.00 107.00   1.00    7.50    --  111.00-111.00  30.00   27
 22  \w     58.00 108.00   1.00    7.50    --  111.00-111.00-180.00   50
 23  \w     45.00  70.00   1.00    7.50    --  111.00 -92.00 -90.00   25
 24  \w     74.00 109.00   1.00    7.50    --  111.00-111.00  60.00   35
 25  \w     81.00 114.00   1.00    7.50    --  111.00 -25.00 -90.00   33
 26  \w    100.00 157.00   1.00    7.50    --  111.00  12.00-150.00   57
 27  \w    111.00 137.00   1.00    7.50    --  111.00 178.00 -30.00   26
 28  \w     85.00 111.00   1.00    7.50    --  111.00 155.00  18.00   26
 29  \w    123.00 155.00   1.00    7.50    --  111.00 155.00  18.00   32
 30  \w     83.00 109.00   1.00    7.50    --  111.00-111.00 -30.00   26
 31  \w    104.00 153.00   1.00    7.50    --  111.00  25.00 -30.00   49
 32  \w     43.00  75.00   1.00    7.50    --  111.00 -25.00 -90.00   32
 33  \w     97.00 123.00   1.00    7.50    --  111.00 -64.00 -30.00   26
 34  \w     42.00 127.00   1.00    7.50    --  111.00 -38.00-180.00   85
 35  \w     76.00 102.00   1.00    7.50    --  111.00 -92.00  60.00   26
 36  \w    119.00 147.00   1.00    7.50    --  111.00 -12.00 -30.00   28
 37  \w     47.00 105.00   1.00    7.50    --  111.00 -12.00 -30.00   58
 38  \w     43.00 102.00   1.00    7.50    --  111.00 -50.00  30.00   59
 39  \w    103.00 128.00   1.00    7.50    --  111.00 -50.00 -30.00   25
 40  \w     50.00 128.00   1.00    7.50    --  111.00 -50.00  90.00   78
 41  \w    138.00 163.00   1.00    7.50    --  111.00  38.00-150.00   25
 42  \w     43.00  68.00   1.00    7.50    --  111.00 -77.00-150.00   25
 43  \w     90.00 129.00   1.00    7.50    --  111.00 -77.00-150.00   39
 44  \w     79.00 109.00   1.00    7.50    --  111.00-111.00 -60.00   30
 45  \w     43.00  89.00   1.00    7.50    --  111.00 -50.00 -30.00   46
 46  \w     75.00 109.00   1.00    7.50    --  111.00-111.00 120.00   34
 47  \w    106.00 143.00   1.00    7.50    --  111.00  50.00-150.00   37
 48  \w     86.00 112.00   1.00    7.50    --  111.00  25.00 150.00   26
 49  \w    132.00 178.00   1.00    7.50    --  111.00  25.00 150.00   46
 50  \w    110.00 135.00   1.00    7.50    --  111.00 -25.00   0.00   25
 51  \w     51.00  99.00   1.00    7.50    --  111.00 -25.00   0.00   48
 52  \w     66.00 109.00   1.00    7.50    --  111.00-111.00 -90.00   43
 53  \w     51.00  77.00   1.00    7.50    --  111.00 -92.00-120.00   26
 54  \w     66.00  91.00   1.00    7.50    --  111.00 -92.00 -60.00   25
 55  \w     45.00  80.00   1.00    7.50    --  111.00 -64.00 -30.00   35
 56  \w    112.00 137.00   1.00    7.50    --  111.00 111.00 -60.00   25
 57  \w    104.00 141.00   1.00    7.50    --  111.00  77.00  30.00   37
 58  \w     95.00 121.00   1.00    7.50    --  111.00 178.00 120.00   26
 59  \w     76.00 101.00   1.00    7.50    --  111.00 -50.00 120.00   25
 60  \w    103.00 177.00   1.00    7.50    --  111.00  64.00-180.00   74
 61  \w    126.00 151.00   1.00    7.50    --  111.00  25.00 -60.00   25
 62  \w     87.00 116.00   1.00    7.50    --  111.00 -77.00  60.00   29
 63  \w     58.00  85.00   1.00    7.50    --  111.00 -31.00  97.02   27
;
_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      -0.0752133000
_diffrn_orient_matrix_UB_12      -0.0033968000
_diffrn_orient_matrix_UB_13      -0.0122207000
_diffrn_orient_matrix_UB_21      0.0008488000
_diffrn_orient_matrix_UB_22      -0.0974415000
_diffrn_orient_matrix_UB_23      0.0169837000
_diffrn_orient_matrix_UB_31      -0.0090357000
_diffrn_orient_matrix_UB_32      0.0191828000
_diffrn_orient_matrix_UB_33      0.0841543000
_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  0.0178
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34915
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.771
_diffrn_reflns_theta_min         3.584
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.863
_exptl_absorpt_correction_T_max  0.55013
_exptl_absorpt_correction_T_min  0.51181
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       prism
_exptl_crystal_F_000             2480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene/n-hexane'
_exptl_crystal_size_max          0.222
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.105
_exptl_crystal_size_rad          0.078
_refine_diff_density_max         0.263
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     418
_refine_ls_number_reflns         5650
_refine_ls_number_restraints     65
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0195
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+3.1376P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0525
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5530
_reflns_number_total             5650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01308e2.cif
_cod_data_source_block           rmk_204_a_scale
_cod_depositor_comments
'Adding full bibliography for 7716434--7716441.cif.'
_cod_database_code               7716439
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C35H25As1Fe1O2 '
_chemical_oxdiff_usercomment     'benzene/pentane at RT '
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-H7 \\sim C0AA-H0AA
 with sigma of 0.02
 C7-C3 \\sim C0AA-C2AA
 with sigma of 0.02
 C7-C6 \\sim C0AA-C1AA
 with sigma of 0.02
 C4-H4 \\sim C3AA-H3AA
 with sigma of 0.02
 C4-C3 \\sim C3AA-C2AA
 with sigma of 0.02
 C4-C5 \\sim C3AA-C0
 with sigma of 0.02
 C3-H3 \\sim C2AA-H2AA
 with sigma of 0.02
 C6-H6 \\sim C1AA-H1AA
 with sigma of 0.02
 C6-C5 \\sim C1AA-C0
 with sigma of 0.02
 C5-H5 \\sim C0-H0
 with sigma of 0.02
 Fe1-C7 \\sim Fe1-C0AA
 with sigma of 0.04
 Fe1-H7 \\sim Fe1-H0AA
 with sigma of 0.04
 Fe1-C4 \\sim Fe1-C3AA
 with sigma of 0.04
 Fe1-H4 \\sim Fe1-H3AA
 with sigma of 0.04
 Fe1-C3 \\sim Fe1-C2AA
 with sigma of 0.04
 Fe1-H3 \\sim Fe1-H2AA
 with sigma of 0.04
 Fe1-C6 \\sim Fe1-C1AA
 with sigma of 0.04
 Fe1-H6 \\sim Fe1-H1AA
 with sigma of 0.04
 Fe1-C5 \\sim Fe1-C0
 with sigma of 0.04
 Fe1-H5 \\sim Fe1-H0
 with sigma of 0.04
 C7-C4 \\sim C0AA-C3AA
 with sigma of 0.04
 C7-H3 \\sim C0AA-H2AA
 with sigma of 0.04
 C7-H6 \\sim C0AA-H1AA
 with sigma of 0.04
 C7-C5 \\sim C0AA-C0
 with sigma of 0.04
 H7-C3 \\sim H0AA-C2AA
 with sigma of 0.04
 H7-C6 \\sim H0AA-C1AA
 with sigma of 0.04
 C4-H3 \\sim C3AA-H2AA
 with sigma of 0.04
 C4-C6 \\sim C3AA-C1AA
 with sigma of 0.04
 C4-H5 \\sim C3AA-H0
 with sigma of 0.04
 H4-C3 \\sim H3AA-C2AA
 with sigma of 0.04
 H4-C5 \\sim H3AA-C0
 with sigma of 0.04
 C3-C6 \\sim C2AA-C1AA
 with sigma of 0.04
 C3-C5 \\sim C2AA-C0
 with sigma of 0.04
 C6-H5 \\sim C1AA-H0
 with sigma of 0.04
 H6-C5 \\sim H1AA-C0
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim
Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
 Sof(H0)=Sof(C0)=Sof(H1AA)=Sof(C1AA)=Sof(C0AA)=Sof(H0AA)=Sof(C2AA)=Sof(H2AA)=
 Sof(C3AA)=Sof(H3AA)=1-FVAR(1)
 Sof(C7)=Sof(H7)=Sof(C4)=Sof(H4)=Sof(C3)=Sof(H3)=Sof(C6)=Sof(H6)=Sof(C5)=
 Sof(H5)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C17(H17), C35(H35), C19(H19), C29(H29), C22(H22), C25(H25),
 C13(H13), C14(H14), C21(H21), C31(H31), C27(H27), C28(H28), C20(H20), C16(H16),
  C15(H15), C34(H34), C26(H26), C32(H32), C7(H7), C33(H33), C4(H4), C3(H3),
 C6(H6), C5(H5)
;
_shelx_res_checksum              47994
_ins_header
;
TITL RMK_204_A_scale in C2/c 
REM C2/c (#15 in standard setting)
CELL 1.54184  20.341822  15.508740  17.765110  90.0000  91.4302  90.0000
ZERR    8.00   0.000126   0.000095   0.000094   0.0000   0.0005   0.0000
LATT  7
SYMM -x, y,-z+1/2 
SFAC C H O Fe As
UNIT 280.00 200.00 16.00 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 1.248
_oxdiff_exptl_absorpt_empirical_full_min 0.841