Synthesis and reactivity of thiolate-bridged multi-iron complexes supported by cyclic (alkyl)(amino)carbene
Zhang, Yanpeng; Mei, Tao; Yang, Dawei; Zhang, Yixin; Wang, Baomin; Qu, Jingping; Dalton Trans.  (2017) –; doi:10.1039/C7DT03353B

data_7044574
_publ_section_title
;
 Synthesis and reactivity of thiolate-bridged multi-iron complexes
 supported by cyclic (alkyl)(amino)carbene
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03353B
_journal_year                    2017
_chemical_formula_moiety         'C42 H68 Fe2 N8 S2'
_chemical_formula_sum            'C42 H68 Fe2 N8 S2'
_chemical_formula_weight         860.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-09-01
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-09-06 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                91.2950(10)
_cell_angle_beta                 104.5310(10)
_cell_angle_gamma                110.9850(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1221(7)
_cell_length_b                   9.6527(8)
_cell_length_c                   14.2111(11)
_cell_measurement_reflns_used    9922
_cell_measurement_temperature    220(2)
_cell_measurement_theta_max      27.280
_cell_measurement_theta_min      3.239
_cell_volume                     1122.17(15)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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_temperature      220.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19905
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.238
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1272 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.6937.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.741
_refine_diff_density_min         -1.134
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4588
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0650
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+2.8551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1594
_refine_ls_wR_factor_ref         0.1641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4104
_reflns_number_total             4588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03353b2.cif
_cod_data_source_block           17jul19cq_0m
_cod_database_code               7044574
_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, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N1-N2
 1.2 with sigma of 0.02
 S1A-Fe1 \\sim Fe1-S1
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N1A) \\sim
Ueq, Uanis(N2A) \\sim Ueq, Uanis(N3A) \\sim Ueq: with sigma of 0.001 and sigma
for terminal atoms of 0.002
Uanis(S1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Fe1, N1, N2, N3, N1A, N2A, N3A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C1, S1, S1A, Fe1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(N1A)=Sof(N2A)=Sof(N3A)=1-FVAR(1)
 Sof(N1)=Sof(N2)=Sof(N3)=FVAR(1)
 Sof(H1BD)=Sof(H1BE)=Sof(H1BF)=Sof(S1A)=1-FVAR(2)
 Sof(S1)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C9(H9), C12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
6.c Me refined with riding coordinates:
 C1(H1AA,H1AB,H1AC), C1(H1BD,H1BE,H1BF)
6.d Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7)
6.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C)
;
_shelx_res_checksum              10925
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'