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_7124462
_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         'C45 H53 As Fe N4 O4'
_chemical_formula_sum            'C45 H53 As Fe N4 O4'
_chemical_formula_weight         844.68
_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_creation_date             2019-08-28
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2019-09-24 deposited with the CCDC.	2019-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.9076(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.33882(14)
_cell_length_b                   20.3971(3)
_cell_length_c                   20.0912(2)
_cell_measurement_reflns_used    28477
_cell_measurement_temperature    100.00(1)
_cell_measurement_theta_max      76.3750
_cell_measurement_theta_min      3.1110
_cell_volume                     4129.81(9)
_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 (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      100.00(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_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    -85.00  -7.00   1.00    4.00    --  -38.50 125.00 150.00   78
  2  \w    -74.00  -7.00   1.00    4.00    --  -38.50 125.00  60.00   67
  3  \w    -86.00 -55.00   1.00    4.00    --  -38.50 125.00 -60.00   31
  4  \w    -58.00  14.00   1.00    4.00    --  -38.50  38.00  90.00   72
  5  \w    -28.00  64.00   1.00    4.00    --   42.89 -38.00 -90.00   92
  6  \w    -22.00  11.00   1.00    4.00    --   42.89 -38.00-180.00   33
  7  \w     26.00 112.00   1.00    4.00    --   42.89  38.00  30.00   86
  8  \w     12.00  42.00   1.00    4.00    --   42.89  80.00  53.15   30
  9  \w     19.00  46.00   1.00    4.00    --   42.89  57.00 150.00   27
 10  \w     28.00  63.00   1.00    4.00    --   42.89 -38.00-180.00   35
 11  \w     13.00  41.00   1.00    4.00    --   42.89  80.00   5.93   28
 12  \w     12.00  41.00   1.00    4.00    --   42.89  82.00-150.43   29
 13  \w     15.00  42.00   1.00    4.00    --   42.89  80.00  80.90   27
 14  \w     26.00 114.00   1.00    4.00    --   42.89  38.00 -30.00   88
 15  \w     21.00 102.00   1.00    4.00    --   42.89  57.00 -90.00   81
 16  \w     22.00  83.00   1.00    4.00    --   42.89  38.00 120.00   61
 17  \w     12.00  42.00   1.00    4.00    --   42.89  82.00 -48.08   30
 18  \w     25.00  94.00   1.00    4.00    --   42.89  38.00-120.00   69
 19  \w     13.00  41.00   1.00    4.00    --   42.89  77.00 -81.18   28
 20  \w     12.00  42.00   1.00    4.00    --   42.89  81.00 144.12   30
 21  \w     48.00  92.00   1.00    4.00    --   42.89  57.00 150.00   44
 22  \w     85.00 112.00   1.00   16.00    --  111.00  60.00 -65.57   27
 23  \w     84.00 113.00   1.00   16.00    --  111.00  66.00  36.59   29
 24  \w     85.00 112.00   1.00   16.00    --  111.00  59.00-151.00   27
 25  \w     83.00 118.00   1.00   16.00    --  111.00  69.00-130.69   35
 26  \w     83.00 110.00   1.00   16.00    --  111.00  67.00-135.92   27
 27  \w    120.00 166.00   1.00   16.00    --  111.00  69.00-130.69   46
 28  \w     35.00 108.00   1.00   16.00    --  111.00-103.00 -12.32   73
 29  \w     79.00 109.00   1.00   16.00    --  111.00-108.00 -64.53   30
 30  \w     82.00 109.00   1.00   16.00    --  111.00  71.00 -27.63   27
 31  \w     85.00 178.00   1.00   16.00    --  111.00  62.00 -37.95   93
 32  \w     83.00 109.00   1.00   16.00    --  111.00  68.00 151.60   26
 33  \w     85.00 111.00   1.00   16.00    --  111.00  61.00 150.00   26
 34  \w    127.00 178.00   1.00   16.00    --  111.00  62.00-163.08   51
 35  \w     90.00 177.00   1.00   16.00    --  111.00  45.00 159.99   87
 36  \w     89.00 118.00   1.00   16.00    --  111.00  43.00  40.12   29
 37  \w     85.00 111.00   1.00   16.00    --  111.00  62.00-163.08   26
 38  \w     82.00 108.00   1.00   16.00    --  111.00  73.00 -58.54   26
 39  \w     86.00 112.00   1.00   16.00    --  111.00  55.00 -71.18   26
 40  \w     49.00 136.00   1.00   16.00    --  111.00 -61.00-180.00   87
 41  \w     85.00 112.00   1.00   16.00    --  111.00  61.00   0.00   27
 42  \w     85.00 173.00   1.00   16.00    --  111.00  61.00 132.52   88
 43  \w     42.00 113.00   1.00   16.00    --  111.00-125.00 150.00   71
 44  \w     85.00 112.00   1.00   16.00    --  111.00  61.00 -30.00   27
 45  \w     85.00 112.00   1.00   16.00    --  111.00  61.00  30.00   27
 46  \w    123.00 178.00   1.00   16.00    --  111.00  61.00  30.00   55
 47  \w     85.00 111.00   1.00   16.00    --  111.00  61.00  90.00   26
 48  \w     84.00 110.00   1.00   16.00    --  111.00  65.00 115.52   26
 49  \w     89.00 160.00   1.00   16.00    --  111.00  45.00 120.00   71
 50  \w     80.00 107.00   1.00   16.00    --  111.00 -94.00  30.00   27
 51  \w    150.00 178.00   1.00   16.00    --  111.00  57.00  87.06   28
 52  \w     85.00 114.00   1.00   16.00    --  111.00  61.00  60.00   29
 53  \w    130.00 178.00   1.00   16.00    --  111.00  61.00  60.00   48
 54  \w     86.00 153.00   1.00   16.00    --  111.00  58.00-108.09   67
 55  \w     85.00 161.00   1.00   16.00    --  111.00  61.00 -60.00   76
 56  \w     43.00 136.00   1.00   16.00    --  111.00 -61.00 -30.00   93
 57  \w     84.00 116.00   1.00   16.00    --  111.00  64.00-146.24   32
 58  \w     85.00 178.00   1.00   16.00    --  111.00  61.00-180.00   93
 59  \w     86.00 112.00   1.00   16.00    --  111.00  57.00  87.06   26
 60  \w     89.00 134.00   1.00   16.00    --  111.00  45.00  90.00   45
 61  \w     85.00 178.00   1.00   16.00    --  111.00  60.00   7.29   93
 62  \w     85.00 111.00   1.00   16.00    --  111.00  59.00-167.32   26
 63  \w     31.00 107.00   1.00   16.00    --  111.00 -94.00-180.00   76
 64  \w     87.00 156.00   1.00   16.00    --  111.00  51.00 -85.96   69
;
_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      0.0689479000
_diffrn_orient_matrix_UB_12      0.0325628000
_diffrn_orient_matrix_UB_13      -0.0519861000
_diffrn_orient_matrix_UB_21      0.0715344000
_diffrn_orient_matrix_UB_22      0.0476744000
_diffrn_orient_matrix_UB_23      0.0556765000
_diffrn_orient_matrix_UB_31      0.1160575000
_diffrn_orient_matrix_UB_32      -0.0487502000
_diffrn_orient_matrix_UB_33      0.0196907000
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79841
_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         76.635
_diffrn_reflns_theta_min         3.128
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.192
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.299
_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
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       plate
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.365
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8652
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0412P)^2^+2.6377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7640
_reflns_number_total             8652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08630g2.cif
_cod_data_source_block           compound7
_cod_original_cell_volume        4129.79(9)
_cod_database_code               7124462
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C164 H192 As4 Fe4 N32 O16 '
_diffrn_oxdiff_digest_frames
;
01d393b1b55d97f9bb87247ec59b02177403112638c
;
_diffrn_oxdiff_digest_hkl
;
01a3eb891dffa0853459c938d663d0e080151d
;
_reflns_odcompleteness_completeness 99.98
_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:
 C19(H19), C22(H22), C31(H31), C34(H34)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C14(H14), C15(H15), C16(H16), C27(H27), C28(H28), C29(H29),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
2.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              475
_olex2_date_sample_data_collection 2019-08-27
_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 2.307
_oxdiff_exptl_absorpt_empirical_full_min 0.465
_oxdiff_exptl_absorpt_spherical_max 0.661
_oxdiff_exptl_absorpt_spherical_min 0.637