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_7127346
_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         'C76 H84 As8 Fe4 N8, 1(C7 H8)'
_chemical_formula_sum            'C83 H92 As8 Fe4 N8'
_chemical_formula_weight         2024.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2020-07-27 deposited with the CCDC.	2020-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.716(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8828(7)
_cell_length_b                   12.9874(3)
_cell_length_c                   26.3513(7)
_cell_measurement_reflns_used    6647
_cell_measurement_temperature    123(1)
_cell_measurement_theta_max      73.8940
_cell_measurement_theta_min      3.3900
_cell_volume                     8272.9(4)
_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 4.1818
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.967
_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   1.00    7.50    --  -44.56  38.00   0.00   76
  2  \w    -50.00  26.00   1.00    7.50    --  -44.56  38.00-120.00   76
  3  \w     82.00 173.00   1.00   30.00    --  104.50  45.00-180.00   91
  4  \w     36.00  98.00   1.00   30.00    --  104.50 -45.00 150.00   62
  5  \w     32.00  91.00   1.00   30.00    --  104.50 -30.00 -60.00   59
  6  \w     36.00  98.00   1.00   30.00    --  104.50 -45.00  60.00   62
  7  \w     81.00 177.00   1.00   30.00    --  104.50  30.00 -90.00   96
  8  \w     32.00  91.00   1.00   30.00    --  104.50 -30.00   0.00   59
  9  \w   -116.00 -14.00   1.00    7.50    --  -44.56 -77.00 -90.00  102
 10  \w     21.00 114.00   1.00    7.50    --   44.56  57.00  90.00   93
 11  \w     33.00  79.00   1.00   30.00    --  104.50-125.00   0.00   46
;
_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      0.0438546000
_diffrn_orient_matrix_UB_12      -0.0820777000
_diffrn_orient_matrix_UB_13      -0.0027989000
_diffrn_orient_matrix_UB_21      0.0000066000
_diffrn_orient_matrix_UB_22      -0.0353521000
_diffrn_orient_matrix_UB_23      0.0558056000
_diffrn_orient_matrix_UB_31      -0.0462531000
_diffrn_orient_matrix_UB_32      -0.0780146000
_diffrn_orient_matrix_UB_33      -0.0223218000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0505
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            22193
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.607
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'gradient vaccum rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.439
_exptl_absorpt_correction_T_max  0.517
_exptl_absorpt_correction_T_min  0.425
_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    1.625
_exptl_crystal_description       block
_exptl_crystal_F_000             4056
_exptl_crystal_recrystallization_method 'from saturated toluene/Et2O solution'
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.107
_refine_diff_density_max         0.577
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         8197
_refine_ls_number_restraints     456
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0346
_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^)+(0.0271P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0667
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6357
_reflns_number_total             8197
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc05173j2.cif
_cod_data_source_block           fs283_1_abs
_cod_depositor_comments
'Adding full bibliography for 7127343--7127347.cif.'
_cod_database_code               7127346
_chemical_oxdiff_formula         'C76 H84 As8 Fe4 N8 (C7H8)'
_reflns_odcompleteness_completeness 99.47
_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. Restrained distances
 C46-C47
 1.51 with sigma of 0.02
 C39-C40
 1.51 with sigma of 0.02
 C47-C48 \\sim C48-C49 \\sim C49-C50 \\sim C50-C51 \\sim C51-C52 \\sim C52-C47
 with sigma of 0.02
 C47-C51 \\sim C47-C49 \\sim C52-C50 \\sim C48-C52 \\sim C49-C51 \\sim C48-C50
 with sigma of 0.04
 C46-C52 \\sim C46-C48
 with sigma of 0.04
 C40-C45 \\sim C45-C44 \\sim C44-C43 \\sim C43-C42 \\sim C42-C41 \\sim C41-C40
 with sigma of 0.02
 C40-C42 \\sim C40-C44 \\sim C41-C43 \\sim C45-C41 \\sim C44-C42 \\sim C45-C43
 with sigma of 0.04
 C39-C41 \\sim C39-C45
 with sigma of 0.04
3. Restrained planarity
 C46, C47, C48, C49, C50, C51, C52
 with sigma of 0.1
 C39, C40, C45, C44, C43, C42, C41
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C39 \\sim C40 \\sim C45 \\sim C44 \\sim C43 \\sim C42 \\sim C41: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C39 \\sim C40 \\sim C45 \\sim C44 \\sim C43 \\sim C42 \\sim C41 \\sim C46 \\sim
C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C51) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C48)
\\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq:
with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C46) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C51) \\sim Ueq, Uanis(C52) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C48) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Rigid body (RIGU) restrains
 C46, C47, C48, C49, C50, C51, C52
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C39, C40, C45, C44, C43, C42, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=Sof(C47)=Sof(C48)=Sof(H48)=Sof(C49)=
 Sof(H49)=Sof(C50)=Sof(H50)=Sof(C51)=Sof(H51)=Sof(C52)=Sof(H52)=0.5*(1-FVAR(2))
 Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=Sof(C45)=Sof(H45)=Sof(C44)=
 Sof(H44)=Sof(C43)=Sof(H43)=Sof(C42)=Sof(H42)=Sof(C41)=Sof(H41)=0.5*FVAR(2)
7.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C20(H20), C35(H35), C21(H21), C3(H3), C33(H33), C34(H34), C1(H1),
 C16(H16), C25(H25), C27(H27), C6(H6), C2(H2), C15(H15), C14(H14), C26(H26),
 C8(H8), C7(H7), C45(H45), C44(H44), C43(H43), C42(H42), C41(H41), C48(H48),
 C49(H49), C50(H50), C51(H51), C52(H52)
7.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C37(H37A,H37B,H37C), C30(H30A,H30B,H30C), C11(H11A,H11B,
 H11C), C19(H19A,H19B,H19C), C18(H18A,H18B,H18C), C10(H10A,H10B,H10C), C29(H29A,
 H29B,H29C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C)
;
_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 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.813