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_7124461
_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         'C40 H45 As Fe N2 O4, 0.5[C4H8O]'
_chemical_formula_sum            'C42 H49 As Fe N2 O4.5'
_chemical_formula_weight         784.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2019-07-12 deposited with the CCDC.	2019-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6009(18)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4632(3)
_cell_length_b                   10.6939(2)
_cell_length_c                   40.9108(8)
_cell_measurement_reflns_used    18676
_cell_measurement_temperature    100.01(11)
_cell_measurement_theta_max      31.0060
_cell_measurement_theta_min      1.9650
_cell_volume                     7912.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.56a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.56a (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      100.01(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.949
_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    -43.00  47.00   1.00   27.50    --   26.03 -57.00-150.00   90
  2  \w      6.00  95.00   1.00   27.50    --   26.03  57.00 -90.00   89
  3  \w     -4.00  42.00   1.00   27.50    --   26.03  77.00-180.00   46
  4  \w     -4.00  42.00   1.00   27.50    --   26.03  77.00  60.00   46
  5  \w    -43.00  47.00   1.00   27.50    --   26.03 -57.00 120.00   90
  6  \w      1.00  98.00   1.00   27.50    --   26.03  38.00 120.00   97
  7  \w      1.00  98.00   1.00   27.50    --   26.03  38.00-150.00   97
  8  \w    -43.00  47.00   1.00   27.50    --   26.03 -57.00  30.00   90
  9  \w    -15.00  68.00   1.00   27.50    --   26.03 -99.00 -30.00   83
 10  \w    -15.00  68.00   1.00   27.50    --   26.03 -99.00-180.00   83
 11  \w      6.00  95.00   1.00   27.50    --   26.03  57.00   0.00   89
 12  \w    -15.00  16.00   1.00   27.50    --   26.03 -99.00   0.00   31
 13  \w     -4.00  42.00   1.00   27.50    --   26.03  77.00 -60.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0351179000
_diffrn_orient_matrix_UB_12      -0.0294369000
_diffrn_orient_matrix_UB_13      -0.0033505000
_diffrn_orient_matrix_UB_21      -0.0156178000
_diffrn_orient_matrix_UB_22      0.0528100000
_diffrn_orient_matrix_UB_23      0.0065290000
_diffrn_orient_matrix_UB_31      -0.0076476000
_diffrn_orient_matrix_UB_32      0.0274269000
_diffrn_orient_matrix_UB_33      -0.0160994000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            92870
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.203
_diffrn_reflns_theta_min         1.971
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.652
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.56a (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 red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       needle
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.449
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         13251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0725
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0491P)^2^+11.6440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1192
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9708
_reflns_number_total             13251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08630g2.cif
_cod_data_source_block           compound4
_cod_original_formula_sum        'C42 H49 As Fe N2 O4.50'
_cod_database_code               7124461
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C37 H45 As Fe N2 O4'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.603
_diffrn_oxdiff_digest_frames
;
01375045839c893cff2ca02ca67bec34f4010199dfc
;
_diffrn_oxdiff_digest_hkl
;
014ede366c69b207706c4bb92d7a26f507f82b
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_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. Uiso/Uaniso restraints and constraints
Uanis(C13B) = Uanis(C13)
3. Others
 Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15B)=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(1)
 Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=
 Sof(H15B)=Sof(H15C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C10(H10), C22(H22), C25(H25), C13(H13), C13B(H13B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36)
4.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14B(H14D,H14E,H14F),
 C15B(H15D,H15E,H15F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              23323
_shelx_fab_checksum              5869
_olex2_date_sample_data_collection 2019-06-24
_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 1.555
_oxdiff_exptl_absorpt_empirical_full_min 0.732