Electrophilic terminal arsinidene-iron(0) complexes with a two-coordinated arsenic atom
Ghadwal, Rajendra S.; Sharma, Mahendra; Neumann, Beate; Stammler, Georg; Andrada, Diego M.; Chemical Communications  (2019) –; doi:10.1039/C9CC08630G

data_7124459
_publ_section_title
;
 Electrophilic terminal arsinidene-iron(0) complexes with a
 two-coordinated arsenic atom
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC08630G
_journal_year                    2019
_chemical_formula_moiety         'C36 H46 N2'
_chemical_formula_sum            'C36 H46 N2'
_chemical_formula_weight         506.75
_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             2018-10-31
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-12 deposited with the CCDC.	2019-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                95.703(4)
_cell_angle_beta                 94.597(4)
_cell_angle_gamma                90.041(4)
_cell_formula_units_Z            4
_cell_length_a                   10.1696(5)
_cell_length_b                   17.3936(8)
_cell_length_c                   18.8594(8)
_cell_measurement_reflns_used    6440
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      76.0570
_cell_measurement_theta_min      4.6950
_cell_volume                     3308.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(13)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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    -62.00  28.00   1.00    3.00    --  -38.50  57.00  60.00   90
  2  \w    -60.00  30.00   1.00    3.00    --  -38.50  57.00 150.00   90
  3  \w     14.00  45.00   1.00    3.00    --   43.45  80.00-140.27   31
  4  \w     76.00 104.00   1.00    3.00    --   43.45  57.00 150.00   28
  5  \w     17.00 115.00   1.00    3.00    --   43.45  77.00   0.00   98
  6  \w     18.00  95.00   1.00    3.00    --   43.45  57.00 -90.00   77
  7  \w     13.00  78.00   1.00    3.00    --   43.45  77.00 150.00   65
  8  \w     33.00  82.00   1.00    3.00    --   43.45 -99.00-180.00   49
  9  \w     18.00  53.00   1.00    3.00    --   43.45  57.00 150.00   35
 10  \w     14.00  78.00   1.00    3.00    --   43.45  77.00  60.00   64
 11  \w     84.00 112.00   1.00    3.00    --   43.45  77.00 150.00   28
 12  \w     24.00 119.00   1.00    3.00    --   43.45  19.00 120.00   95
 13  \w     13.00  95.00   1.00    3.00    --   43.45  77.00 -60.00   82
 14  \w      3.00  66.00   1.00    3.00    --   43.45 -99.00 -60.00   63
 15  \w     31.00 110.00   1.00   12.00    --  111.00 -94.00  90.00   79
 16  \w     41.00  86.00   1.00   12.00    --  111.00-125.00  90.00   45
 17  \w     81.00 107.00   1.00   12.00    --  111.00  76.00 -36.40   26
 18  \w     81.00 106.00   1.00   12.00    --  111.00  77.00-150.00   25
 19  \w    121.00 178.00   1.00   12.00    --  111.00  77.00   0.00   57
 20  \w     82.00 107.00   1.00   12.00    --  111.00  71.00  39.90   25
 21  \w     84.00 111.00   1.00   12.00    --  111.00  63.00  39.03   27
 22  \w     81.00 106.00   1.00   12.00    --  111.00  77.00   0.00   25
 23  \w     81.00 106.00   1.00   12.00    --  111.00  77.00  60.00   25
 24  \w     85.00 111.00   1.00   12.00    --  111.00  61.00 -60.00   26
 25  \w     45.00  91.00   1.00   12.00    --  111.00 -77.00-120.00   46
 26  \w     85.00 177.00   1.00   12.00    --  111.00  61.00  60.00   92
 27  \w     81.00 107.00   1.00   12.00    --  111.00  77.00 120.00   26
 28  \w     93.00 118.00   1.00   12.00    --  111.00-125.00  90.00   25
 29  \w     85.00 111.00   1.00   12.00    --  111.00  61.00  30.00   26
 30  \w     58.00 118.00   1.00   12.00    --  111.00-125.00 -30.00   60
 31  \w     85.00 120.00   1.00   12.00    --  111.00  61.00  90.00   35
 32  \w    128.00 160.00   1.00   12.00    --  111.00  61.00-180.00   32
 33  \w     85.00 111.00   1.00   12.00    --  111.00  61.00 120.00   26
 34  \w     83.00 108.00   1.00   12.00    --  111.00  68.00 -90.72   25
 35  \w     85.00 122.00   1.00   12.00    --  111.00  61.00-180.00   37
 36  \w     85.00 178.00   1.00   12.00    --  111.00  61.00 -30.00   93
 37  \w     81.00 107.00   1.00   12.00    --  111.00  77.00 150.00   26
 38  \w     81.00 107.00   1.00   12.00    --  111.00  77.00-180.00   26
 39  \w     81.00 178.00   1.00   12.00    --  111.00  77.00  90.00   97
 40  \w     81.00 107.00   1.00   12.00    --  111.00  77.00 -30.00   26
 41  \w     85.00 177.00   1.00   12.00    --  111.00  61.00-120.00   92
 42  \w     85.00 177.00   1.00   12.00    --  111.00  61.00 -90.00   92
 43  \w     56.00 117.00   1.00   12.00    --  111.00-125.00  60.00   61
 44  \w     43.00 134.00   1.00   12.00    --  111.00 -61.00  90.00   91
 45  \w    112.00 171.00   1.00   12.00    --  111.00  77.00 120.00   59
 46  \w     81.00 107.00   1.00   12.00    --  111.00  77.00 -90.00   26
 47  \w     81.00 171.00   1.00   12.00    --  111.00  77.00 -60.00   90
 48  \w     85.00 175.00   1.00   12.00    --  111.00  61.00 150.00   90
 49  \w     81.00 106.00   1.00   12.00    --  111.00  77.00-120.00   25
 50  \w     85.00 160.00   1.00   12.00    --  111.00  61.00-150.00   75
 51  \w     85.00 129.00   1.00   12.00    --  111.00  61.00   0.00   44
 52  \w    115.00 157.00   1.00   12.00    --  111.00  63.00  39.03   42
 53  \w    100.00 138.00   1.00   12.00    --  111.00 -77.00-120.00   38
 54  \w     81.00 118.00   1.00   12.00    --  111.00-125.00-120.00   37
 55  \w     83.00 109.00   1.00   12.00    --  111.00  69.00  89.28   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1294770000
_diffrn_orient_matrix_UB_12      -0.0464291000
_diffrn_orient_matrix_UB_13      -0.0017366000
_diffrn_orient_matrix_UB_21      -0.0795868000
_diffrn_orient_matrix_UB_22      0.0739685000
_diffrn_orient_matrix_UB_23      -0.0102267000
_diffrn_orient_matrix_UB_31      0.0003628000
_diffrn_orient_matrix_UB_32      -0.0172223000
_diffrn_orient_matrix_UB_33      -0.0817052000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1009
_diffrn_reflns_av_unetI/netI     0.0734
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58682
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.126
_diffrn_reflns_theta_min         2.362
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.437
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.017
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.101
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         13017
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.3073P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1571
_refine_ls_wR_factor_ref         0.1882
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7705
_reflns_number_total             13017
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08630g2.cif
_cod_data_source_block           (MeIPr)CHPh
_cod_database_code               7124459
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C48(H48), C51(H51), C60(H60), C63(H63)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C44(H44), C45(H45), C46(H46), C56(H56),
  C57(H57), C58(H58), C66(H66), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,
 H64C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              93375
_shelx_fab_checksum              27654
_olex2_date_sample_data_collection 2018-10-30
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.330
_oxdiff_exptl_absorpt_empirical_full_min 0.727