Free and Coordinated Biarsolyls
Hill, Anthony; Kirk, Ryan M.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02070C

data_7713701
_publ_section_title
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 Free and Coordinated Biarsolyls
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02070C
_journal_year                    2023
_chemical_formula_moiety         'C23 H22 As Fe Mo O5, F6 P'
_chemical_formula_sum            'C23 H22 As F6 Fe Mo O5 P'
_chemical_formula_weight         750.08
_chemical_properties_physical    Air-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_block_doi                 10.5517/ccdc.csd.cc2b0ftm
_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.	2023-07-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.707(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6104(11)
_cell_length_b                   14.7837(7)
_cell_length_c                   13.7151(12)
_cell_measurement_reflns_used    4668
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.8380
_cell_measurement_theta_min      4.4080
_cell_volume                     2711.6(4)
_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  (Sheldrick, 2015)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.977
_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    -98.00 -37.00   1.00   12.00    --  -36.18 -38.00 -90.00   61
  2  \w     29.00  88.00   1.00   12.00    --   36.18-125.00 -30.00   59
  3  \w     39.00  91.00   1.00   12.00    --   36.18  57.00-150.00   52
  4  \w     48.00  89.00   1.00   12.00    --   36.18-125.00-180.00   41
  5  \w    -33.00  54.00   1.00   12.00    --   36.18 -38.00  90.00   87
  6  \w     18.00 104.00   1.00   12.00    --   36.18  19.00 -60.00   86
  7  \w     17.00 105.00   1.00   12.00    --   36.18  38.00  30.00   88
  8  \w      7.00  63.00   1.00   12.00    --   36.18 -99.00  60.00   56
  9  \w     42.00 125.00   1.00   25.00    --  109.99 -45.00-180.00   83
 10  \w     42.00 126.00   1.00   25.00    --  109.99 -45.00  90.00   84
 11  \w     58.00 129.00   1.00   25.00    --  109.99 -77.00-120.00   71
 12  \w     43.00 127.00   1.00   25.00    --  109.99 -45.00 -90.00   84
 13  \w     47.00 109.00   1.00   25.00    --  109.99-111.00-120.00   62
 14  \w     41.00 109.00   1.00   25.00    --  109.99-111.00  60.00   68
 15  \w     43.00 106.00   1.00   25.00    --  109.99 -95.00 120.00   63
 16  \w    111.00 165.00   1.00   25.00    --  109.99  45.00 150.00   54
 17  \w     46.00 126.00   1.00   25.00    --  109.99 -45.00   0.00   80
 18  \w     41.00 178.00   1.00   25.00    --  109.99   0.00 120.00  137
;
_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      -0.0816773000
_diffrn_orient_matrix_UB_12      0.0507882000
_diffrn_orient_matrix_UB_13      0.0421939000
_diffrn_orient_matrix_UB_21      0.0580234000
_diffrn_orient_matrix_UB_22      -0.0161091000
_diffrn_orient_matrix_UB_23      0.1062231000
_diffrn_orient_matrix_UB_31      0.0566214000
_diffrn_orient_matrix_UB_32      0.0895878000
_diffrn_orient_matrix_UB_33      -0.0048010000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5784
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.580
_diffrn_reflns_theta_min         4.202
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.674
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75261
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/Et2O'
_refine_diff_density_max         2.537
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5784
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0743
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1458P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2143
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4066
_reflns_number_total             5784
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.7610\% 
 around [0.70 -0.00 0.72] (reciprocal) or [0.71 -0.00 0.71] (direct)
;
_cod_data_source_file            d3dt02070c2.cif
_cod_data_source_block           rmk_219_d_scaletwin_twin1_hklf4
_cod_database_code               7713701
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         Mo1Fe1As1P1F6C20H15O3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.47(7)
 0.35(3) 0.18(6)
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:
 C20(H20), C21(H21), C16(H16), C13(H13), C12(H12), C19(H19), C22(H22),
 C14(H14), C23(H23), C15(H15)
3.b Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C11(H11a,H11b,H11c), C10(H10a,H10b,H10c)
;
_shelx_res_checksum              25292
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.613
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2