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_7124463
_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         'C38 H41 As Fe N2 O4'
_chemical_formula_sum            'C38 H41 As Fe N2 O4'
_chemical_formula_weight         720.50
_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             2019-11-04
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_audit_update_record
;
2019-11-04 deposited with the CCDC.	2019-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                81.8399(16)
_cell_angle_beta                 87.3548(19)
_cell_angle_gamma                85.871(2)
_cell_formula_units_Z            4
_cell_length_a                   10.5768(3)
_cell_length_b                   17.8360(4)
_cell_length_c                   21.1952(4)
_cell_measurement_reflns_used    35314
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      76.3930
_cell_measurement_theta_min      3.4680
_cell_volume                     3945.06(16)
_computing_cell_refinement       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.58a (Rigaku OD, 2019)'
_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 n/a (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_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 0.977
_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    -84.00  -6.00   1.00    5.00    --  -38.50 125.00  60.00   78
  2  \w    -44.00  19.00   1.00    5.00    --  -38.50  57.00  60.00   63
  3  \w    -70.00  24.00   1.00    5.00    --  -38.50  19.00   0.00   94
  4  \w     12.00  39.00   1.00    5.00    --   42.89  80.00  36.81   27
  5  \w     14.00  41.00   1.00    5.00    --   42.89  82.00 166.18   27
  6  \w     22.00  82.00   1.00    5.00    --   42.89  38.00  60.00   60
  7  \w     45.00  93.00   1.00    5.00    --   42.89  66.00 -28.18   48
  8  \w     29.00  80.00   1.00    5.00    --   42.89 -99.00 -30.00   51
  9  \w     14.00  40.00   1.00    5.00    --   42.89  78.00 116.75   26
 10  \w     18.00  63.00   1.00    5.00    --   42.89  57.00-120.00   45
 11  \w     73.00 101.00   1.00    5.00    --   42.89  57.00-120.00   28
 12  \w     17.00  80.00   1.00    5.00    --   42.89  70.00  81.00   63
 13  \w    -28.00  64.00   1.00    5.00    --   42.89 -38.00 150.00   92
 14  \w     18.00 111.00   1.00    5.00    --   42.89  57.00-180.00   93
 15  \w     14.00 108.00   1.00    5.00    --   42.89  70.00 -75.71   94
 16  \w     15.00  41.00   1.00    5.00    --   42.89  66.00 -28.18   26
 17  \w     13.00  38.00   1.00    5.00    --   42.89  76.00 -14.08   25
 18  \w     82.00 178.00   1.00   18.00    --  111.00  73.00-164.89   96
 19  \w     86.00 112.00   1.00   18.00    --  111.00  56.00  19.26   26
 20  \w     82.00 108.00   1.00   18.00    --  111.00  71.00 162.21   26
 21  \w    148.00 178.00   1.00   18.00    --  111.00  72.00  69.61   30
 22  \w     43.00 106.00   1.00   18.00    --  111.00 -94.00 -30.00   63
 23  \w     40.00 123.00   1.00   18.00    --  111.00 -77.00  90.00   83
 24  \w     82.00 108.00   1.00   18.00    --  111.00  72.00  69.61   26
 25  \w     85.00 110.00   1.00   18.00    --  111.00  61.00 150.00   25
 26  \w    126.00 158.00   1.00   18.00    --  111.00  61.00 150.00   32
 27  \w     41.00 113.00   1.00   18.00    --  111.00-125.00 -90.00   72
 28  \w     85.00 111.00   1.00   18.00    --  111.00  61.00 -30.00   26
 29  \w     89.00 133.00   1.00   18.00    --  111.00  45.00 120.00   44
 30  \w     85.00 160.00   1.00   18.00    --  111.00  61.00  30.00   75
 31  \w    127.00 174.00   1.00   18.00    --  111.00  60.00-131.54   47
 32  \w     82.00 108.00   1.00   18.00    --  111.00  72.00 112.49   26
 33  \w     46.00 133.00   1.00   18.00    --  111.00 -45.00  90.00   87
 34  \w     85.00 111.00   1.00   18.00    --  111.00  61.00   0.00   26
 35  \w     88.00 141.00   1.00   18.00    --  111.00  47.00  63.71   53
 36  \w     85.00 117.00   1.00   18.00    --  111.00  61.00-120.00   32
 37  \w     90.00 116.00   1.00   18.00    --  111.00  45.00 150.00   26
 38  \w    147.00 173.00   1.00   18.00    --  111.00  61.00  90.00   26
 39  \w     31.00 105.00   1.00   18.00    --  111.00 -94.00 -90.00   74
 40  \w    119.00 178.00   1.00   18.00    --  111.00  59.00-100.79   59
 41  \w     85.00 111.00   1.00   18.00    --  111.00  60.00-131.54   26
 42  \w     85.00 111.00   1.00   18.00    --  111.00  61.00  90.00   26
 43  \w     89.00 121.00   1.00   18.00    --  111.00  45.00-150.00   32
 44  \w     85.00 111.00   1.00   18.00    --  111.00  61.00 120.00   26
 45  \w    125.00 165.00   1.00   18.00    --  111.00  61.00 -60.00   40
 46  \w     85.00 121.00   1.00   18.00    --  111.00  61.00 -60.00   36
 47  \w     89.00 169.00   1.00   18.00    --  111.00  45.00-180.00   80
 48  \w     87.00 113.00   1.00   18.00    --  111.00  54.00 -68.52   26
 49  \w     85.00 112.00   1.00   18.00    --  111.00  59.00-100.79   27
 50  \w     89.00 177.00   1.00   18.00    --  111.00  45.00   0.00   88
 51  \w     85.00 111.00   1.00   18.00    --  111.00  61.00-180.00   26
 52  \w     32.00 107.00   1.00   18.00    --  111.00 -94.00  60.00   75
 53  \w     85.00 173.00   1.00   18.00    --  111.00  61.00  60.00   88
 54  \w     86.00 111.00   1.00   18.00    --  111.00  56.00 -62.64   25
 55  \w     85.00 114.00   1.00   18.00    --  111.00  61.00 -90.00   29
 56  \w     84.00 110.00   1.00   18.00    --  111.00  66.00 -13.02   26
 57  \w     34.00 106.00   1.00   18.00    --  111.00-100.00  28.00   72
 58  \w     87.00 178.00   1.00   18.00    --  111.00  54.00 -36.99   91
 59  \w    113.00 178.00   1.00   18.00    --  111.00  72.00 112.49   65
;
_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      -0.1155250000
_diffrn_orient_matrix_UB_12      -0.0486829000
_diffrn_orient_matrix_UB_13      0.0120940000
_diffrn_orient_matrix_UB_21      -0.0143951000
_diffrn_orient_matrix_UB_22      0.0186313000
_diffrn_orient_matrix_UB_23      0.0688552000
_diffrn_orient_matrix_UB_31      -0.0883236000
_diffrn_orient_matrix_UB_32      0.0702152000
_diffrn_orient_matrix_UB_33      -0.0226166000
_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  0.0606
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            72562
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.267
_diffrn_reflns_theta_min         2.508
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.288
_exptl_absorpt_correction_T_max  0.798
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.58a (Rigaku Oxford Diffraction, 2019)
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 black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.229
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     845
_refine_ls_number_reflns         16360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0356
_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^)+(0.0507P)^2^+1.0104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14713
_reflns_number_total             16360
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08630g2.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        3945.04(16)
_cod_database_code               7124463
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         AsC39Cl2FeH43N2O4
_shelx_estimated_absorpt_t_max   0.704
_shelx_estimated_absorpt_t_min   0.440
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.024) H3(0.026) H6(0.03) H7(0.032) H8(0.03) H10(0.026)
 H11A(0.047) H11B(0.047) H11C(0.047) H12A(0.045) H12B(0.045) H12C(0.045)
 H13(0.03) H14A(0.048) H14B(0.048) H14C(0.048) H15A(0.05) H15B(0.05) H15C(0.05)
 H18(0.038) H19(0.042) H20(0.035) H22(0.035) H23A(0.063) H23B(0.063)
 H23C(0.063) H24A(0.058) H24B(0.058) H24C(0.058) H25(0.027) H26A(0.046)
 H26B(0.046) H26C(0.046) H27A(0.049) H27B(0.049) H27C(0.049) H30(0.032)
 H31(0.045) H32(0.055) H33(0.052) H34(0.036) H40(0.026) H41(0.024) H44(0.044)
 H45(0.047) H46(0.042) H48(0.036) H49A(0.059) H49B(0.059) H49C(0.059)
 H50A(0.064) H50B(0.064) H50C(0.064) H51(0.035) H52A(0.061) H52B(0.061)
 H52C(0.061) H53A(0.061) H53B(0.061) H53C(0.061) H56(0.026) H57(0.028)
 H58(0.026) H60(0.024) H61A(0.039) H61B(0.039) H61C(0.039) H62A(0.036)
 H62B(0.036) H62C(0.036) H63(0.025) H64A(0.044) H64B(0.044) H64C(0.044)
 H65A(0.056) H65B(0.056) H65C(0.056) H68(0.033) H69(0.045) H70(0.046)
 H71(0.042) H72(0.032)
 Fixed X: H2(0.212727) H3(0.186012) H6(-0.026049) H7(0.166024) H8(0.345231)
 H10(-0.082246) H11A(-0.079545) H11B(-0.222616) H11C(-0.153229) H12A(-0.207271)
 H12B(-0.268911) H12C(-0.156127) H13(0.352188) H14A(0.38734) H14B(0.515168)
 H14C(0.485371) H15A(0.503014) H15B(0.542607) H15C(0.426632) H18(0.28252)
 H19(0.124308) H20(-0.041283) H22(0.294901) H23A(0.401839) H23B(0.501177)
 H23C(0.465958) H24A(0.411952) H24B(0.427559) H24C(0.29541) H25(-0.1065) H26A(-
 0.045092) H26B(-0.128022) H26C(0.019144) H27A(-0.234509) H27B(-0.287164) H27C(-
 0.212527) H30(-0.181711) H31(-0.35712) H32(-0.341541) H33(-0.148348)
 H34(0.027179) H40(0.304473) H41(0.29086) H44(0.232476) H45(0.40889)
 H46(0.568087) H48(0.176272) H49A(0.205881) H49B(0.05848) H49C(0.116669)
 H50A(0.0349) H50B(-0.022793) H50C(0.074562) H51(0.587231) H52A(0.73624)
 H52B(0.788304) H52C(0.741794) H53A(0.480161) H53B(0.627908) H53C(0.572379)
 H56(0.207589) H57(0.408827) H58(0.588565) H60(0.134528) H61A(0.021355) H61B(-
 0.035941) H61C(0.085497) H62A(0.125426) H62B(-0.01344) H62C(0.067738)
 H63(0.58954) H64A(0.690202) H64B(0.79001) H64C(0.752788) H65A(0.676963)
 H65B(0.728985) H65C(0.585506) H68(0.539945) H69(0.440429) H70(0.223465)
 H71(0.104235) H72(0.20133)
 Fixed Y: H2(0.508047) H3(0.528793) H6(0.607766) H7(0.628116) H8(0.647357)
 H10(0.605838) H11A(0.48629) H11B(0.520863) H11C(0.523672) H12A(0.665033)
 H12B(0.663394) H12C(0.717218) H13(0.662438) H14A(0.764022) H14B(0.730922)
 H14C(0.707988) H15A(0.570506) H15B(0.588734) H15C(0.53705) H18(0.786042)
 H19(0.769074) H20(0.693354) H22(0.710767) H23A(0.617676) H23B(0.668776)
 H23C(0.682947) H24A(0.818936) H24B(0.80883) H24C(0.842162) H25(0.614533)
 H26A(0.529129) H26B(0.499919) H26C(0.512594) H27A(0.695635) H27B(0.613677)
 H27C(0.63131) H30(0.700152) H31(0.752674) H32(0.861861) H33(0.919104)
 H34(0.868015) H40(0.034658) H41(0.026021) H44(0.266994) H45(0.225638)
 H46(0.145531) H48(0.220303) H49A(0.347899) H49B(0.335179) H49C(0.339147)
 H50A(0.21129) H50B(0.205691) H50C(0.139629) H51(0.087045) H52A(0.094644)
 H52B(0.066702) H52C(0.153876) H53A(-0.008394) H53B(-0.033555) H53C(-0.001836)
 H56(0.174709) H57(0.170322) H58(0.150434) H60(0.167295) H61A(0.212194)
 H61B(0.230341) H61C(0.271762) H62A(0.042539) H62B(0.084606) H62C(0.075134)
 H63(0.12622) H64A(0.224311) H64B(0.160081) H64C(0.160924) H65A(0.029409)
 H65B(0.022451) H65C(0.004913) H68(0.332684) H69(0.424249) H70(0.457503)
 H71(0.394334) H72(0.300632)
 Fixed Z: H2(0.285486) H3(0.16865) H6(0.4832) H7(0.52431) H8(0.457763)
 H10(0.31663) H11A(0.380978) H11B(0.372592) H11C(0.437654) H12A(0.4236)
 H12B(0.356299) H12C(0.361284) H13(0.286364) H14A(0.345139) H14B(0.312788)
 H14C(0.387472) H15A(0.380759) H15B(0.306668) H15C(0.328772) H18(0.017242) H19(-
 0.050529) H20(-0.01419) H22(0.183105) H23A(0.1268) H23B(0.152437)
 H23C(0.078886) H24A(0.090469) H24B(0.166004) H24C(0.136209) H25(0.146809)
 H26A(0.043459) H26B(0.106014) H26C(0.111366) H27A(0.069285) H27B(0.090961)
 H27C(0.023665) H30(0.2345) H31(0.177041) H32(0.103585) H33(0.086849)
 H34(0.144876) H40(0.265873) H41(0.383136) H44(0.082574) H45(0.024298)
 H46(0.074046) H48(0.252062) H49A(0.206988) H49B(0.221217) H49C(0.149862)
 H50A(0.141618) H50B(0.213145) H50C(0.192888) H51(0.24281) H52A(0.126135)
 H52B(0.195843) H52C(0.17586) H53A(0.20289) H53B(0.208952) H53C(0.140614)
 H56(0.563416) H57(0.603723) H58(0.538536) H60(0.400928) H61A(0.516414)
 H61B(0.446908) H61C(0.463028) H62A(0.455992) H62B(0.455694) H62C(0.518544)
 H63(0.372987) H64A(0.414883) H64B(0.39351) H64C(0.467464) H65A(0.484237)
 H65B(0.413055) H65C(0.433744) H68(0.396633) H69(0.454197) H70(0.44477)
 H71(0.381753) H72(0.326034)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              76707
_shelx_fab_checksum              49870
_olex2_date_sample_data_collection 2019-10-31
_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 2.092
_oxdiff_exptl_absorpt_empirical_full_min 0.376