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_7124460
_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 H45 As Cl2 N2, 0.5(C6 H6)'
_chemical_formula_sum            'C39 H48 As Cl2 N2'
_chemical_formula_weight         690.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-15
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_audit_update_record
;
2019-07-12 deposited with the CCDC.	2019-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.448(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4516(5)
_cell_length_b                   9.0396(2)
_cell_length_c                   17.9260(4)
_cell_measurement_reflns_used    11609
_cell_measurement_temperature    100.00(11)
_cell_measurement_theta_max      30.4010
_cell_measurement_theta_min      2.2910
_cell_volume                     3506.71(14)
_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      100.00(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.927
_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    -13.00  97.00   1.00    7.26    --   24.78  19.00-180.00  110
  2  \w    -44.00  43.00   1.00    7.26    --   24.78 -57.00   0.00   87
  3  \w      6.00  93.00   1.00    7.26    --   24.78  57.00-120.00   87
  4  \w    -44.00  53.00   1.00    7.26    --   24.78 -77.00-180.00   97
  5  \w     -4.00  94.00   1.00    7.26    --   24.78  77.00 120.00   98
  6  \w    -20.00  65.00   1.00    7.26    --   24.78 -99.00 -60.00   85
  7  \w     -4.00  26.00   1.00    7.26    --   24.78  77.00 -60.00   30
;
_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      0.0290165000
_diffrn_orient_matrix_UB_12      0.0052780000
_diffrn_orient_matrix_UB_13      -0.0085285000
_diffrn_orient_matrix_UB_21      -0.0139200000
_diffrn_orient_matrix_UB_22      0.0408154000
_diffrn_orient_matrix_UB_23      -0.0339640000
_diffrn_orient_matrix_UB_31      0.0062112000
_diffrn_orient_matrix_UB_32      0.0667995000
_diffrn_orient_matrix_UB_33      0.0214284000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51545
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.258
_diffrn_reflns_theta_min         1.882
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.151
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.636
_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    1.308
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1452
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.192
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.806
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         11539
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0262P)^2^+2.8226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8523
_reflns_number_total             11539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc08630g2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        3506.70(14)
_cod_database_code               7124460
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C39 H48 As Cl2 N2'
_reflns_odcompleteness_completeness 99.97
_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. Restrained distances
 C13-C12 \\sim C13B-C12B \\sim C14B-C12 \\sim C14-C12B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C12B) = Uanis(C12)
4. Others
 Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(C14B)=
 Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(1)
 Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14D)=
 Sof(H14E)=Sof(H14F)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C12B(H12B), C15(H15), C24(H24), C27(H27)
5.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39)
5.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C13B(H13D,H13E,H13F),
 C14(H14D,H14E,H14F), C14B(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)
;
_shelx_res_checksum              96225
_olex2_date_sample_data_collection 2018-11-15
_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 1.114
_oxdiff_exptl_absorpt_empirical_full_min 0.853