Iron β-diiminate complexes with As<sub>2</sub>-, As<sub>4</sub>- and As<sub>8</sub>-ligands.
Spitzer, Fabian; Balázs, Gábor; Graßl, Christian; Scheer, Manfred; Chemical communications (Cambridge, England) 56 (2020) 13209–13212; doi:10.1039/d0cc05173j

data_7127347
_publ_section_title
;
 Iron \b-diiminate complexes with As<sub>2</sub>-, As<sub>4</sub>- and
 As<sub>8</sub>-ligands.
;
_journal_issue                   86
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              13209
_journal_page_last               13212
_journal_paper_doi               10.1039/d0cc05173j
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         'C58 H82 As3.78 Fe2 N4'
_chemical_formula_sum            'C58 H82 As3.78 Fe2 N4'
_chemical_formula_weight         1229.79
_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             2016-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2884(2)
_cell_length_b                   13.60190(10)
_cell_length_c                   15.3559(2)
_cell_measurement_reflns_used    30741
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.4830
_cell_measurement_theta_min      3.1970
_cell_volume                     2897.28(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      123(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3636
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9892
_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     22.00  85.00   1.00    2.00    --   44.81  38.00   0.00   63
  2  \w     92.00 138.00   1.00    2.00    --   72.00  77.00 -28.55   46
  3  \w    110.00 160.00   1.00   10.00    --   92.00  72.00 -32.51   50
  4  \w    142.00 175.00   1.00   10.00    --  104.50  77.00 -30.00   33
  5  \w    144.00 170.00   1.00   10.00    --  104.50  77.00-150.00   26
  6  \w    113.00 172.00   1.00   10.00    --  104.50  77.00  30.00   59
  7  \w    114.00 140.00   1.00    2.00    --   72.00  67.00 143.70   26
  8  \w    107.00 175.00   1.00   10.00    --  104.50  77.00  60.00   68
  9  \w     76.00 167.00   1.00   10.00    --  104.50  84.00 -90.04   91
 10  \w     75.00 161.00   1.00   10.00    --  104.50  77.00 -60.00   86
 11  \w     77.00 113.00   1.00   10.00    --  104.50  69.00  58.22   36
 12  \w     75.00 100.00   1.00   10.00    --  104.50  77.00  60.00   25
 13  \w     74.00 176.00   1.00   10.00    --  104.50  77.00  90.00  102
 14  \w     74.00 162.00   1.00   10.00    --  104.50  77.00-120.00   88
 15  \w     74.00 140.00   1.00   10.00    --  104.50  77.00-150.00   66
 16  \w     74.00 174.00   1.00   10.00    --  104.50  77.00-180.00  100
 17  \w     75.00 149.00   1.00   10.00    --  104.50  77.00   0.00   74
 18  \w     74.00 174.00   1.00   10.00    --  104.50  77.00 150.00  100
 19  \w     75.00 122.00   1.00   10.00    --  104.50  77.00 -30.00   47
 20  \w     74.00 100.00   1.00   10.00    --  104.50  77.00  30.00   26
 21  \w     63.00  89.00   1.00   10.00    --   92.00  72.00 -32.51   26
 22  \w     74.00  99.00   1.00   10.00    --  104.50  77.00 -90.00   25
 23  \w     56.00  82.00   1.00   10.00    --   84.00  69.00-147.41   26
 24  \w     44.00  71.00   1.00    2.00    --   72.00  77.00 -96.71   27
 25  \w     49.00  75.00   1.00   10.00    --   76.00  69.00 -72.38   26
 26  \w     42.00  69.00   1.00    2.00    --   72.00  77.00 -28.55   27
 27  \w     48.00  77.00   1.00   10.00    --   76.00  74.00   3.84   29
 28  \w     54.00 108.00   1.00    2.00    --   44.81  64.00  57.99   54
 29  \w     50.00  76.00   1.00   10.00    --   80.00  75.00 178.24   26
 30  \w     45.00  71.00   1.00    2.00    --   72.00  67.00 143.70   26
 31  \w     38.00  64.00   1.00    2.00    --   68.00  77.00 117.72   26
 32  \w     42.00  68.00   1.00    2.00    --   72.00  77.00  63.60   26
 33  \w     47.00  73.00   1.00   10.00    --   76.00  74.00  39.26   26
 34  \w     35.00  60.00   1.00    2.00    --   64.00  76.00  93.63   25
 35  \w     27.00  54.00   1.00    2.00    --   56.00  75.00  27.23   27
 36  \w     19.00  45.00   1.00    2.00    --   44.81  64.00  57.99   26
 37  \w     20.00  45.00   1.00    2.00    --   52.00  81.00  69.00   25
 38  \w      6.00  31.00   1.00    2.00    --   40.00  90.00   9.64   25
 39  \w     35.00  60.00   1.00    2.00    --   64.00  75.00 -31.18   25
 40  \w     38.00  64.00   1.00    2.00    --   68.00  75.00 -99.95   26
 41  \w     34.00  61.00   1.00    2.00    --   64.00  77.00-133.33   27
 42  \w     23.00 100.00   1.00    2.00    --   44.81  38.00-120.00   77
 43  \w     21.00  46.00   1.00    2.00    --   52.00  79.00-118.30   25
 44  \w     20.00  45.00   1.00    2.00    --   52.00  81.00 -59.24   25
 45  \w     17.00  92.00   1.00    2.00    --   44.81  19.00-180.00   75
 46  \w     41.00 126.00   1.00   10.00    --  104.50 -77.00 -30.00   85
 47  \w     95.00 121.00   1.00   10.00    --  104.50-125.00  60.00   26
 48  \w     49.00 102.00   1.00   10.00    --  104.50 -94.00 -90.00   53
 49  \w     41.00 131.00   1.00    2.00    --   44.81-178.00  30.00   90
 50  \w     40.00 107.00   1.00   10.00    --  104.50 -94.00 120.00   67
 51  \w     27.00  53.00   1.00    2.00    --   56.00  75.00 178.69   26
 52  \w     39.00  64.00   1.00    2.00    --   68.00  76.00 177.96   25
 53  \w     74.00 150.00   1.00   10.00    --  104.50  77.00 120.00   76
 54  \w     31.00  64.00   1.00   10.00    --  104.50 -94.00-120.00   33
 55  \w     39.00 108.00   1.00   10.00    --  104.50 -94.00-180.00   69
 56  \w    -25.00  69.00   1.00    2.00    --   44.81 -57.00  60.00   94
 57  \w      7.00  23.00   1.00    2.00    --   40.00  86.00 165.74   16
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, TitanS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1078169000
_diffrn_orient_matrix_UB_12      0.0065077000
_diffrn_orient_matrix_UB_13      -0.0473033000
_diffrn_orient_matrix_UB_21      -0.0056846000
_diffrn_orient_matrix_UB_22      0.1016922000
_diffrn_orient_matrix_UB_23      0.0425705000
_diffrn_orient_matrix_UB_31      0.0258497000
_diffrn_orient_matrix_UB_32      0.0494030000
_diffrn_orient_matrix_UB_33      -0.0814876000
_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  0.0319
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            53667
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.815
_diffrn_reflns_theta_min         3.797
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.698
_exptl_absorpt_correction_T_max  0.418
_exptl_absorpt_correction_T_min  0.260
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
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            'dark black'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       block
_exptl_crystal_F_000             1403.680
_exptl_crystal_recrystallization_method 'from saturated Et2O solution'
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.205
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5889
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0503P)^2^+2.5878P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5807
_reflns_number_total             5889
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05173j2.cif
_cod_data_source_block           fs284wh2_mp_abs
_cod_depositor_comments
'Adding full bibliography for 7127343--7127347.cif.'
_cod_database_code               7127347
_chemical_oxdiff_formula         C58H82N4Fe2As3.76
_chemical_oxdiff_usercomment     'black block'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C28A) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(As4) \\sim Ueq, Uanis(As5) \\sim Ueq, Uanis(As3) \\sim Ueq: with sigma of
0.002 and sigma for terminal atoms of 0.002
3. Others
 Sof(As3)=Sof(As5)=Sof(As4)=0.5*(1-FVAR(2))
 Sof(As2)=Sof(As1)=FVAR(1)
 Fixed Sof: H27(0.581) H27A(0.419) H24(0.421) H24A(0.579) C25(0.421)
 H25A(0.421) H25B(0.421) H25C(0.421) C28(0.581) H28A(0.581) H28B(0.581)
 H28C(0.581) C28A(0.419) H28D(0.419) H28E(0.419) H28F(0.419) C25A(0.579)
 H25D(0.579) H25E(0.579) H25F(0.579)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C27(H27), C27(H27A), C24(H24), C24(H24A)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C8(H8), C9(H9), C20(H20), C22(H22), C21(H21)
4.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C1(H1A,H1B,H1C),
 C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C16(H16A,H16B,
 H16C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F),
 C25A(H25D,H25E,H25F)
;
_shelx_shelxl_version_number     2016/6
_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 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.807