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_7127343
_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         '2(C27 H37 As2 Fe N2)'
_chemical_formula_sum            'C54 H74 As4 Fe2 N4'
_chemical_formula_weight         1190.55
_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             2017-02-06
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.02.06 svn.r3384 for OlexSys, GUI svn.r5312)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                89.203(4)
_cell_angle_beta                 87.031(4)
_cell_angle_gamma                67.239(5)
_cell_formula_units_Z            2
_cell_length_a                   13.2431(6)
_cell_length_b                   13.9354(8)
_cell_length_c                   16.0383(7)
_cell_measurement_reflns_used    14345
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      74.2620
_cell_measurement_theta_min      3.3650
_cell_volume                     2725.6(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.982
_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     21.00  78.00   0.50    1.00    --   44.08  38.00 -90.00  114
  2  \w     84.00 111.00   0.50    1.00    --   44.08  38.00 -90.00   54
  3  \w    108.00 176.00   0.50    8.00    --  104.50  77.00   0.00  136
  4  \w    124.00 172.00   0.50    8.00    --  104.50  61.00  30.00   96
  5  \w    107.00 176.00   0.50    8.00    --  104.50  77.00 -30.00  138
  6  \w    122.00 149.00   0.50    8.00    --  104.50  77.00-120.00   54
  7  \w     79.00 105.00   0.50    8.00    --  104.50  61.00-120.00   52
  8  \w     80.00 107.00   0.50    8.00    --  104.50  61.00-150.00   54
  9  \w     75.00 102.00   0.50    8.00    --  104.50  77.00-180.00   54
 10  \w     74.00 175.00   0.50    8.00    --  104.50  77.00-150.00  202
 11  \w     79.00 121.00   0.50    8.00    --  104.50  61.00 -30.00   84
 12  \w     79.00 174.00   0.50    8.00    --  104.50  61.00  60.00  190
 13  \w     79.00 138.00   0.50    8.00    --  104.50  61.00 -90.00  118
 14  \w     79.00 107.00   0.50    8.00    --  104.50  61.00  30.00   56
 15  \w     79.00 107.00   0.50    8.00    --  104.50  61.00   0.00   56
 16  \w     74.00 100.00   0.50    8.00    --  104.50  77.00   0.00   52
 17  \w     74.00 100.00   0.50    8.00    --  104.50  77.00 -30.00   52
 18  \w     74.00 100.00   0.50    8.00    --  104.50  77.00 -60.00   52
 19  \w     74.00 100.00   0.50    8.00    --  104.50  77.00 -90.00   52
 20  \w     74.00 100.00   0.50    8.00    --  104.50  77.00-120.00   52
 21  \w     74.00 172.00   0.50    8.00    --  104.50  77.00 -77.62  196
 22  \w     80.00 172.00   0.50    8.00    --  104.50  61.00 120.00  184
 23  \w     74.00 129.00   0.50    8.00    --  104.50  77.00 150.00  110
 24  \w     79.00 105.00   0.50    8.00    --  104.50  61.00 150.00   52
 25  \w     74.00 100.00   0.50    8.00    --  104.50  77.00 120.00   52
 26  \w     79.00 155.00   0.50    8.00    --  104.50  61.00  90.00  152
 27  \w     76.00 155.00   0.50    8.00    --  104.50  71.00 170.44  158
 28  \w     74.00 100.00   0.50    8.00    --  104.50  77.00  30.00   52
 29  \w     74.00 100.00   0.50    8.00    --  104.50  77.00  60.00   52
 30  \w     74.00 101.00   0.50    8.00    --  104.50  77.00  90.00   54
 31  \w     45.00  93.00   0.50    1.00    --   44.08 167.00  15.00   96
 32  \w     14.00  99.00   0.50    1.00    --   44.08  77.00   0.00  170
 33  \w     20.00  58.00   0.50    1.00    --   44.08  57.00  90.00   76
 34  \w     16.00 110.00   0.50    1.00    --   44.08  77.00 150.00  188
 35  \w     14.00  97.00   0.50    1.00    --   44.08  77.00  90.00  166
 36  \w     15.00 116.00   0.50    1.00    --   44.08  77.00 -90.00  202
 37  \w     50.00  95.00   0.50    8.00    --  104.50 -45.00 -60.00   90
 38  \w     56.00 119.00   0.50    8.00    --  104.50-125.00 -30.00  126
 39  \w     34.00 129.00   0.50    1.00    --   44.08-178.00 -90.00  190
 40  \w     24.00 109.00   0.50    8.00    --  104.50 -94.00 -30.00  170
 41  \w     31.00 114.00   0.50    8.00    --  104.50-116.00 140.00  166
 42  \w     34.00 133.00   0.50    8.00    --  104.50 -77.00 150.00  198
 43  \w     23.00  95.00   0.50    8.00    --  104.50 -94.00  60.00  144
 44  \w     16.00  46.00   0.50    1.00    --   44.08  77.00-150.00   60
 45  \w   -130.00 -40.00   0.50    1.00    --  -44.08 178.00 -90.00  180
;
_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      -0.0184679000
_diffrn_orient_matrix_UB_12      -0.0111668000
_diffrn_orient_matrix_UB_13      0.0946603000
_diffrn_orient_matrix_UB_21      0.1245229000
_diffrn_orient_matrix_UB_22      -0.0574218000
_diffrn_orient_matrix_UB_23      0.0078620000
_diffrn_orient_matrix_UB_31      0.0103944000
_diffrn_orient_matrix_UB_32      0.1046488000
_diffrn_orient_matrix_UB_33      0.0151493000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            45715
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.322
_diffrn_reflns_theta_min         2.759
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.246
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.606
_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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_recrystallization_method 'from saturated Et2O solution'
_exptl_crystal_size_max          0.101
_exptl_crystal_size_mid          0.079
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.448
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         10933
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0879P)^2^+1.8752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1461
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9491
_reflns_number_total             10933
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05173j2.cif
_cod_data_source_block           fs265_abs
_cod_depositor_comments
'Adding full bibliography for 7127343--7127347.cif.'
_cod_original_cell_volume        2725.6(2)
_cod_database_code               7127343
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C54H74As4Fe2N4
_chemical_oxdiff_usercomment     'brown 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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N4) \\sim Ueq, Uanis(N4A) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C30A)
\\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C29A) \\sim Ueq, Uanis(C28) \\sim Ueq,
Uanis(C28A) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
3. Others
 Sof(N3)=Sof(N4)=Sof(C28)=Sof(H28)=Sof(C30)=Sof(H30)=Sof(C29)=Sof(H29)=
 Sof(As6)=Sof(As5)=Sof(Fe2B)=1-FVAR(1)
 Sof(Fe2A)=Sof(As3)=Sof(As4)=Sof(N3A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29A)=
 Sof(C30A)=Sof(H30A)=Sof(N4A)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C10(H10), C22(H22), C25(H25), C40(H40), C52(H52), C49(H49), C37(H37)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C1(H1), C8(H8), C2(H2), C7(H7), C20(H20), C18(H18), C19(H19),
 C28(H28), C30(H30), C29(H29), C45(H45), C47(H47), C33(H33), C35(H35), C46(H46),
  C34(H34), C28A(H28A), C29A(H29A), C30A(H30A)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C12(H12A,H12B,
 H12C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C51(H51A,H51B,H51C),
 C50(H50A,H50B,H50C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C39(H39A,H39B,
 H39C), C38(H38A,H38B,H38C)
;
_shelx_res_checksum              52820
_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 1.579
_oxdiff_exptl_absorpt_empirical_full_min 0.671