Metallodithiolates as ligands to dinitrosyl iron complexes: toward the understanding of structures, equilibria, and spin coupling.
Pinder, Tiffany A.; Montalvo, Steven K.; Hsieh, Chung-Hung; Lunsford, Allen M.; Bethel, Ryan D.; Pierce, Brad S.; Darensbourg, Marcetta Y.; Inorganic chemistry 53 (2014) 9095–9105; doi:10.1021/ic501117f

data_4340884
_publ_section_title
;
 Metallodithiolates as ligands to dinitrosyl iron complexes: toward the
 understanding of structures, equilibria, and spin coupling.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9095
_journal_page_last               9105
_journal_paper_doi               10.1021/ic501117f
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C10 H20 Fe2 I2 N6 Ni O4 S2'
_chemical_formula_sum            'C10 H20 Fe2 I2 N6 Ni O4 S2'
_chemical_formula_weight         776.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 91.237(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.274(3)
_cell_length_b                   15.992(5)
_cell_length_c                   13.674(4)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    110.15
_cell_measurement_theta_max      28.19
_cell_measurement_theta_min      2.36
_cell_volume                     2246.1(12)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0410
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26133
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.353
_diffrn_reflns_theta_min         2.357
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.066
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1125 before and 0.0569 after correction.
The Ratio of minimum to maximum transmission is 0.6867.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.297
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         5560
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0304
_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^)+(0.0208P)^2^+6.1338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4888
_reflns_number_total             5560
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic501117f_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4340882--4340885.cif.'
_cod_original_cell_volume        2246.2(11)
_cod_database_code               4340884
_shelx_estimated_absorpt_t_max   0.606
_shelx_estimated_absorpt_t_min   0.462
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 I1-N3 = I1A-N3A
 3.649 with sigma of 0.005
 I1-O1 = I1A-O1A
 4.665 with sigma of 0.005
 Fe1-O1 = Fe1A-O1A
 2.781 with sigma of 0.005
 Fe1-N3 = Fe1A-N3A
 1.713 with sigma of 0.005
 S2-C10 \\sim S2-C10A
 with sigma of 0.005
 C9A-C10A \\sim C9-C10
 with sigma of 0.005
 N2-C9 \\sim N2-C9A
 with sigma of 0.005
 N2-C5 \\sim N2-C5A \\sim N1-C3 \\sim N1-C3A
 with sigma of 0.005
 C4-C3 \\sim C4A-C3A \\sim C5A-C4A \\sim C5-C4
 with sigma of 0.005
 I1-Fe1 \\sim I1A-Fe1A
 with sigma of 0.005
 Fe1-S1 \\sim Fe1A-S1
 with sigma of 0.005
 I1A-Fe1A \\sim I1-Fe1
 with sigma of 0.005
 Fe1-N4 \\sim Fe1A-N4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C9A) = Uanis(C9)
Uanis(C10A) = Uanis(C10)
Uanis(C5A) = Uanis(C5) = Uanis(C3) = Uanis(C3A)
Uanis(C4A) = Uanis(C4)
Uanis(I1A) = Uanis(I1)
Uanis(Fe1A) = Uanis(Fe1)
Uanis(N3) = Uanis(N3A)
Uanis(O1) = Uanis(O1A)
4. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=
 Sof(H5AB)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(C10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(Fe1A)=Sof(I1A)=Sof(N3A)=Sof(O1A)=1-FVAR(2)
 Sof(I1)=Sof(Fe1)=Sof(O1)=Sof(N3)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C3A(H3AA,H3AB),
 C4A(H4AA,H4AB), C5A(H5AA,H5AB), C9A(H9AA,H9AB), C10A(H10C,H10D)
;
_shelx_res_checksum              80854
_shelx_hkl_checksum              3677