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_7127344
_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             2017-02-13
_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                89.309(2)
_cell_angle_beta                 86.365(2)
_cell_angle_gamma                67.800(3)
_cell_formula_units_Z            2
_cell_length_a                   13.2706(5)
_cell_length_b                   14.0867(5)
_cell_length_c                   15.8705(3)
_cell_measurement_reflns_used    31148
_cell_measurement_temperature    122.97(14)
_cell_measurement_theta_max      74.3790
_cell_measurement_theta_min      2.6930
_cell_volume                     2741.13(16)
_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      122.97(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3636
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.956
_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    -50.00  26.00   0.50    5.00    --  -44.81  38.00  90.00  152
  2  \w   -131.00 -34.00   0.50    5.00    --  -44.81 178.00-180.00  194
  3  \w   -124.00 -79.00   0.50    5.00    --  -44.81 -99.00  60.00   90
  4  \w    -50.00  26.00   0.50    5.00    --  -44.81  38.00-180.00  152
  5  \w     14.00 117.00   0.50    5.00    --   44.81  77.00-180.00  206
  6  \w     14.00 117.00   0.50    5.00    --   44.81  77.00-120.00  206
  7  \w     14.00 117.00   0.50    5.00    --   44.81  77.00  60.00  206
  8  \w     14.00 117.00   0.50    5.00    --   44.81  77.00 120.00  206
  9  \w     22.00 115.00   0.50    5.00    --   44.81  38.00   0.00  186
 10  \w     14.00 117.00   0.50    5.00    --   44.81  77.00 -30.00  206
 11  \w     79.00 174.00   0.50   30.00    --  104.50  61.00  30.00  190
 12  \w     74.00 176.00   0.50   30.00    --  104.50  77.00 120.00  204
 13  \w     79.00 174.00   0.50   30.00    --  104.50  61.00   0.00  190
 14  \w     79.00 174.00   0.50   30.00    --  104.50  61.00 120.00  190
 15  \w     79.00 174.00   0.50   30.00    --  104.50  61.00  90.00  190
 16  \w     74.00 177.00   0.50   30.00    --  104.50  78.00-139.12  206
 17  \w     79.00 174.00   0.50   30.00    --  104.50  61.00 150.00  190
 18  \w     33.00 121.00   0.50   30.00    --  104.50-125.00-180.00  176
 19  \w     74.00 176.00   0.50   30.00    --  104.50  77.00   0.00  204
 20  \w     33.00 135.00   0.50   30.00    --  104.50 -77.00 120.00  204
 21  \w     74.00  99.00   0.50   30.00    --  104.50  77.00 -30.00   50
 22  \w    112.00 171.00   0.50   30.00    --  104.50  77.00 -30.00  118
 23  \w     74.00  99.00   0.50   30.00    --  104.50  77.00  90.00   50
 24  \w     79.00 104.00   0.50   30.00    --  104.50  61.00 -30.00   50
 25  \w    114.00 174.00   0.50   30.00    --  104.50  77.00  30.00  120
 26  \w    120.00 146.00   0.50   30.00    --  104.50  77.00  60.00   52
 27  \w     74.00 100.00   0.50   30.00    --  104.50  77.00  60.00   52
 28  \w     74.00  99.00   0.50   30.00    --  104.50  77.00  30.00   50
 29  \w     74.00  99.00   0.50   30.00    --  104.50  77.00 -90.00   50
 30  \w     74.00 100.00   0.50   30.00    --  104.50  77.00-150.00   52
 31  \w     80.00 110.00   0.50   30.00    --  104.50  61.00-180.00   60
 32  \w     74.00  99.00   0.50   30.00    --  104.50  77.00-180.00   50
 33  \w    125.00 172.00   0.50   30.00    --  104.50  77.00-180.00   94
 34  \w     79.00 117.00   0.50   30.00    --  104.50  61.00  60.00   76
 35  \w     79.00 174.00   0.50   30.00    --  104.50  61.00 -90.00  190
 36  \w     74.00 100.00   0.50   30.00    --  104.50  77.00-120.00   52
 37  \w     74.00 169.00   0.50   30.00    --  104.50  77.00 -60.00  190
 38  \w     33.00 121.00   0.50   30.00    --  104.50-125.00 -30.00  176
 39  \w     33.00 135.00   0.50   30.00    --  104.50 -77.00 -30.00  204
 40  \w     77.00 103.00   0.50   30.00    --  104.50  68.00 -63.40   52
 41  \w     74.00 172.00   0.50   30.00    --  104.50  77.00 150.00  196
 42  \w     77.00 127.00   0.50   30.00    --  104.50  67.00-153.66  100
;
_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      0.0023053000
_diffrn_orient_matrix_UB_12      0.0346539000
_diffrn_orient_matrix_UB_13      0.0913127000
_diffrn_orient_matrix_UB_21      0.0805656000
_diffrn_orient_matrix_UB_22      -0.1084155000
_diffrn_orient_matrix_UB_23      0.0199682000
_diffrn_orient_matrix_UB_31      0.0963759000
_diffrn_orient_matrix_UB_32      0.0316143000
_diffrn_orient_matrix_UB_33      -0.0269368000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49210
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.902
_diffrn_reflns_theta_min         2.790
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.205
_exptl_absorpt_correction_T_max  0.562
_exptl_absorpt_correction_T_min  0.387
_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    1.442
_exptl_crystal_description       block
_exptl_crystal_F_000             1220
_exptl_crystal_recrystallization_method 'from saturated Et2O solution'
_exptl_crystal_size_max          0.215
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.134
_refine_diff_density_max         1.275
_refine_diff_density_min         -1.321
_refine_diff_density_rms         0.141
_refine_ls_extinction_coef       0.00052(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         10940
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1441P)^2^+2.0205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1880
_refine_ls_wR_factor_ref         0.1984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10205
_reflns_number_total             10940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05173j2.cif
_cod_data_source_block           fs294_abs_rint03
_cod_depositor_comments
'Adding full bibliography for 7127343--7127347.cif.'
_cod_database_code               7127344
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C54 H74 N4 Fe2 As4'
_chemical_oxdiff_usercomment     'black block'
_reflns_odcompleteness_completeness 99.26
_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(N4A) \\sim Ueq, Uanis(N4) \\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(As6)=Sof(Fe2B)=Sof(As5)=Sof(N4A)=Sof(C30A)=Sof(H30A)=Sof(C29A)=Sof(H29A)=
 Sof(C28A)=Sof(H28A)=Sof(N3A)=1-FVAR(1)
 Sof(Fe2A)=Sof(As3)=Sof(N4)=Sof(N3)=Sof(C30)=Sof(H30)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29)=Sof(As4)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C13(H13), C37(H37), C40(H40), C10(H10), C49(H49), C22(H22), C52(H52), C25(H25)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C1(H1), C30(H30), C3(H3), C2(H2), C28(H28), C29(H29), C35(H35),
 C33(H33), C7(H7), C34(H34), C8(H8), C47(H47), C46(H46), C45(H45), C20(H20),
 C18(H18), C19(H19), C30A(H30A), C29A(H29A), C28A(H28A)
4.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C), C39(H39A,H39B,H39C), C38(H38A,H38B,
 H38C), C41(H41A,H41B,H41C), C11(H11A,H11B,H11C), C51(H51A,H51B,H51C), C42(H42A,
 H42B,H42C), C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C50(H50A,H50B,H50C),
 C23(H23A,H23B,H23C), C53(H53A,H53B,H53C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              86884
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 1.699
_oxdiff_exptl_absorpt_empirical_full_min 0.762