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_7127345
_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         'C84 H100 As8 Fe4 N8, 2.5(C7 H8)'
_chemical_formula_sum            'C101.5 H120 As8 Fe4 N8'
_chemical_formula_weight         2274.81
_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             2016-12-19
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                82.1763(8)
_cell_angle_beta                 76.4461(8)
_cell_angle_gamma                78.1144(8)
_cell_formula_units_Z            2
_cell_length_a                   13.60288(12)
_cell_length_b                   14.75365(14)
_cell_length_c                   26.0325(2)
_cell_measurement_reflns_used    20321
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.4800
_cell_measurement_theta_min      3.3860
_cell_volume                     4948.88(8)
_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      123.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5431
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.9853
_diffrn_measured_fraction_theta_max 0.9690
_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     17.00 105.00   0.50    4.00    --   41.44  38.00  30.00  176
  2  \w    -33.00  68.00   0.50    4.00    --   41.44 -38.00-150.00  202
  3  \w     -6.00  74.00   0.50    4.00    --   41.44 -77.00  90.00  160
  4  \w     25.00 112.00   0.50   15.00    --   93.50 -80.00  23.00  174
  5  \w    123.00 168.00   0.50   15.00    --   93.50  45.00 -90.00   90
  6  \w     19.00  72.00   0.50   15.00    --   93.50 -45.00  30.00  106
  7  \w     68.00 103.00   0.50   15.00    --   93.50  45.00 -90.00   70
  8  \w     34.00  85.00   0.50   15.00    --   93.50  15.00  60.00  102
  9  \w    115.00 177.00   0.50   15.00    --   93.50  15.00  60.00  124
 10  \w     13.00 113.00   0.50   15.00    --   93.50 -80.00 116.00  200
 11  \w     29.00  68.00   0.50   15.00    --   93.50 -45.00-120.00   78
 12  \w     67.00 168.00   0.50   15.00    --   93.50  45.00-180.00  202
 13  \w     17.00 107.00   0.50   15.00    --   93.50 -80.00 -44.00  180
 14  \w     18.00 109.00   0.50   15.00    --   93.50 -80.00-150.00  182
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0215155000
_diffrn_orient_matrix_UB_12      0.0074665000
_diffrn_orient_matrix_UB_13      -0.0560930000
_diffrn_orient_matrix_UB_21      0.1155270000
_diffrn_orient_matrix_UB_22      -0.0315907000
_diffrn_orient_matrix_UB_23      -0.0226519000
_diffrn_orient_matrix_UB_31      -0.0148459000
_diffrn_orient_matrix_UB_32      -0.1021301000
_diffrn_orient_matrix_UB_33      0.0088302000
_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  0.0245
_diffrn_reflns_av_unetI/netI     0.0320
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            32388
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        66.512
_diffrn_reflns_theta_max         66.512
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.957
_exptl_absorpt_correction_T_max  0.478
_exptl_absorpt_correction_T_min  0.182
_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 red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.527
_exptl_crystal_description       block
_exptl_crystal_F_000             2549.000
_exptl_crystal_size_max          0.318
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1215
_refine_ls_number_reflns         16930
_refine_ls_number_restraints     495
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0279
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+0.9718P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16065
_reflns_number_total             16930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05173j2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7127343--7127347.cif.'
_cod_original_formula_sum        'C101.50 H120 As8 Fe4 N8'
_cod_database_code               7127345
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C101.5H120As8Fe4N8
_cell_oxdiff_angle_alpha         82.1763(8)
_cell_oxdiff_angle_beta          76.4461(8)
_cell_oxdiff_angle_gamma         78.1144(8)
_cell_oxdiff_length_a            13.60288(12)
_cell_oxdiff_length_b            14.75365(14)
_cell_oxdiff_length_c            26.0325(2)
_cell_oxdiff_measurement_reflns_used 20321
_cell_oxdiff_volume              4948.88(8)
_reflns_odcompleteness_completeness 98.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     64.99
_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
 C99-C100
 1.51 with sigma of 0.02
 C106-C107
 1.51 with sigma of 0.02
 C92-C93
 1.51 with sigma of 0.02
 C100-C101 \\sim C101-C102 \\sim C102-C103 \\sim C103-C104 \\sim C104-C105
\\sim C105-C100
 with sigma of 0.02
 C100-C104 \\sim C100-C102 \\sim C105-C103 \\sim C101-C105 \\sim C102-C104
\\sim C101-C103
 with sigma of 0.04
 C99-C105 \\sim C99-C101
 with sigma of 0.04
 C107-C112 \\sim C112-C111 \\sim C111-C110 \\sim C110-C109 \\sim C109-C108
\\sim C108-C107
 with sigma of 0.02
 C107-C109 \\sim C107-C111 \\sim C108-C110 \\sim C112-C108 \\sim C111-C109
\\sim C112-C110
 with sigma of 0.04
 C106-C108 \\sim C106-C112
 with sigma of 0.04
 C93-C94 \\sim C94-C95 \\sim C95-C96 \\sim C96-C97 \\sim C97-C98 \\sim C98-C93
 with sigma of 0.02
 C93-C97 \\sim C93-C95 \\sim C98-C96 \\sim C94-C98 \\sim C95-C97 \\sim C94-C96
 with sigma of 0.04
 C92-C98 \\sim C92-C94
 with sigma of 0.04
3. Restrained planarity
 C99, C100, C101, C102, C103, C104, C105
 with sigma of 0.1
 C106, C107, C112, C111, C110, C109, C108
 with sigma of 0.1
 C92, C93, C94, C95, C96, C97, C98
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C99 \\sim C100 \\sim C101 \\sim C102 \\sim C103 \\sim C104 \\sim C105: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C106 \\sim C107 \\sim C112 \\sim C111 \\sim C110 \\sim C109 \\sim C108: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97 \\sim C98: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C103) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C105)
\\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C102) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C108) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq,
Uanis(C105) \\sim Ueq, Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq,
Uanis(C102) \\sim Ueq, Uanis(C100) \\sim Ueq, Uanis(C112) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C101) \\sim Ueq, Uanis(C99) \\sim Ueq, Uanis(C111)
\\sim Ueq, Uanis(C110) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C92) \\sim Ueq, Uanis(C93) \\sim Ueq, Uanis(C94) \\sim Ueq, Uanis(C98)
\\sim Ueq, Uanis(C95) \\sim Ueq, Uanis(C97) \\sim Ueq, Uanis(C96) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 C99, C100, C101, C102, C103, C104, C105
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C106, C107, C112, C111, C110, C109, C108
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C92, C93, C94, C95, C96, C97, C98
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: C99(0.5) H99A(0.5) H99B(0.5) H99C(0.5) C100(0.5) C101(0.5)
 H101(0.5) C102(0.5) H102(0.5) C103(0.5) H103(0.5) C104(0.5) H104(0.5)
 C105(0.5) H105(0.5) C106(0.5) H10A(0.5) H10B(0.5) H10C(0.5) C107(0.5)
 C112(0.5) H112(0.5) C111(0.5) H111(0.5) C110(0.5) H110(0.5) C109(0.5)
 H109(0.5) C108(0.5) H108(0.5) C92(0.5) H92A(0.5) H92B(0.5) H92C(0.5) C93(0.5)
 C94(0.5) H94(0.5) C95(0.5) H95(0.5) C96(0.5) H96(0.5) C97(0.5) H97(0.5)
 C98(0.5) H98(0.5)
7.a Me refined with riding coordinates:
 C99(H99A,H99B,H99C), C106(H10A,H10B,H10C)
7.b Aromatic/amide H refined with riding coordinates:
 C81(H81), C80(H80), C79(H79), C50(H50), C51(H51), C66(H66), C8(H8), C72(H72),
 C71(H71), C10(H10), C37(H37), C31(H31), C73(H73), C52(H52), C24(H24), C9(H9),
 C45(H45), C18(H18), C29(H29), C30(H30), C17(H17), C58(H58), C3(H3), C38(H38),
 C16(H16), C39(H39), C59(H59), C60(H60), C88(H88), C87(H87), C91(H91), C89(H89),
  C90(H90), C101(H101), C102(H102), C103(H103), C104(H104), C105(H105),
 C112(H112), C111(H111), C110(H110), C109(H109), C108(H108), C94(H94), C95(H95),
  C96(H96), C97(H97), C98(H98)
7.c Idealised Me refined as rotating group:
 C83(H83A,H83B,H83C), C26(H26A,H26B,H26C), C76(H76A,H76B,H76C), C84(H84A,H84B,
 H84C), C33(H33A,H33B,H33C), C75(H75A,H75B,H75C), C55(H55A,H55B,H55C), C13(H13A,
 H13B,H13C), C21(H21A,H21B,H21C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C43(H43A,H43B,H43C), C68(H68A,H68B,H68C), C34(H34A,H34B,H34C), C20(H20A,H20B,
 H20C), C12(H12A,H12B,H12C), C62(H62A,H62B,H62C), C5(H5A,H5B,H5C), C42(H42A,
 H42B,H42C), C22(H22A,H22B,H22C), C41(H41A,H41B,H41C), C54(H54A,H54B,H54C),
 C47(H47A,H47B,H47C), C1(H1A,H1B,H1C), C85(H85A,H85B,H85C), C92(H92A,H92B,H92C)
;
_shelx_res_checksum              43595
_olex2_diffrn_ambient_temperature_device 'Oxford Instruments, CryoJet'
_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 1.295
_oxdiff_exptl_absorpt_empirical_full_min 0.868