Diiron Bridged-Thiolate Complexes That Bind N2 at the Fe(II)Fe(II), Fe(II)Fe(I), and Fe(I)Fe(I) Redox States.
Creutz, Sidney E.; Peters, Jonas C.; Journal of the American Chemical Society 137 (2015) 7310–7313; doi:10.1021/jacs.5b04738

data_4123802
_publ_section_title
;
 Diiron Bridged-Thiolate Complexes That Bind N2 at the Fe(II)Fe(II),
 Fe(II)Fe(I), and Fe(I)Fe(I) Redox States.
;
_journal_issue                   23
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7310
_journal_page_last               7313
_journal_paper_doi               10.1021/jacs.5b04738
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C32 H12 B F24, C54 H75 Fe2 N4 P4 S Si2'
_chemical_formula_sum            'C80 H80 B F24 Fe2 N4 O2 P4 S Si2'
_chemical_formula_weight         1920.11
_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
_audit_creation_date             2015-04-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                73.269(2)
_cell_angle_beta                 77.147(2)
_cell_angle_gamma                88.109(2)
_cell_formula_units_Z            2
_cell_length_a                   16.5053(10)
_cell_length_b                   16.6824(10)
_cell_length_c                   18.8438(11)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      2.25
_cell_volume                     4841.8(5)
_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, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1616
_diffrn_reflns_av_unetI/netI     0.1485
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            208905
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.585
_diffrn_reflns_theta_min         1.782
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.501
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0883 before and 0.0609 after correction.
The Ratio of minimum to maximum transmission is 0.8853.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1962
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1195
_refine_ls_number_reflns         29598
_refine_ls_number_restraints     1602
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.1746
_refine_ls_R_factor_gt           0.0805
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+3.4459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1761
_refine_ls_wR_factor_ref         0.2020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14190
_reflns_number_total             29598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04738_si_002.cif
_cod_data_source_block           compound10
_cod_depositor_comments
'Adding full bibliography for 4123801--4123807.cif.'
_cod_database_code               4123802
_shelxl_version_number           2014/6
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(N1) \\sim Ueq, Uanis(N2) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C24A)
\\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(F531) \\sim Ueq, Uanis(F533) \\sim Ueq, Uanis(F532) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.2
Uanis(F534) \\sim Ueq, Uanis(F535) \\sim Ueq, Uanis(F536) \\sim Ueq,
Uanis(C531) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1
Uanis(C111) = Uanis(C115)
Uanis(C113) = Uanis(C116)
Uanis(C123) = Uanis(C126)
Uanis(C21) = Uanis(C21A)
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C15A)
Uanis(C14) = Uanis(C14A)
Uanis(C13) = Uanis(C13A)
Uanis(C12) = Uanis(C12A)
Uanis(C11) = Uanis(C11A)
Uanis(F535) = Uanis(F532)
Uanis(F534) = Uanis(F531)
Uanis(F536) = Uanis(F533)
4. Same fragment restrains
{F534, F535, F536} sigma for 1-2: 0.02, 1-3: 0.04
{F533, F532, F531} sigma for 1-2: 0.02, 1-3: 0.04
{F551, F552, F552} sigma for 1-2: 0.02, 1-3: 0.04
as
{F531, F532, F533}
{C21A, C22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C21, C22, C23, C25, C24, C26}
{C16A, C15A, C14A, C13A, C12A, C11A} sigma for 1-2: 0.02, 1-3: 0.04
as
{C16, C15, C14, C13, C12, C11}
{C114, C115, C116} sigma for 1-2: 0.02, 1-3: 0.04
as
{C113, C111, C112}
{C124, C125, C126} sigma for 1-2: 0.02, 1-3: 0.04
as
{C122, C121, C123}
5. Others
 Sof(C16A)=Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=Sof(C13A)=Sof(H13A)=
 Sof(C12A)=Sof(H12A)=Sof(C11A)=1-FVAR(1)
 Sof(C16)=Sof(C15)=Sof(H15)=Sof(C14)=Sof(H14)=Sof(C13)=Sof(H13)=Sof(C12)=
 Sof(H12)=Sof(C11)=FVAR(1)
 Sof(C114)=Sof(H11G)=Sof(H11H)=Sof(H11I)=Sof(C115)=Sof(H115)=Sof(C116)=
 Sof(H11J)=Sof(H11K)=Sof(H11L)=1-FVAR(2)
 Sof(C113)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C111)=Sof(H111)=Sof(C112)=
 Sof(H11D)=Sof(H11E)=Sof(H11F)=FVAR(2)
 Sof(C124)=Sof(H12H)=Sof(H12I)=Sof(H12J)=Sof(C125)=Sof(H125)=Sof(C126)=
 Sof(H12K)=Sof(H12L)=Sof(H12M)=1-FVAR(3)
 Sof(C122)=Sof(H12B)=Sof(H12C)=Sof(H12D)=Sof(C121)=Sof(H121)=Sof(C123)=
 Sof(H12E)=Sof(H12F)=Sof(H12G)=FVAR(3)
 Sof(C21A)=Sof(C22A)=Sof(H22G)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=
 Sof(C25A)=Sof(H25A)=Sof(C26A)=1-FVAR(4)
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C25)=Sof(H25)=Sof(C24)=
 Sof(H24)=Sof(C26)=FVAR(4)
 Sof(F534)=Sof(F535)=Sof(F536)=1-FVAR(5)
 Sof(F531)=Sof(F532)=Sof(F533)=FVAR(5)
6.a Ternary CH refined with riding coordinates:
 C421(H421), C411(H411), C221(H221), C211(H211), C311(H311), C321(H321),
 C111(H111), C115(H115), C121(H121), C125(H125)
6.b Me refined with riding coordinates:
 C114(H11G,H11H,H11I), C116(H11J,H11K,H11L), C124(H12H,H12I,H12J), C126(H12K,
 H12L,H12M)
6.c Aromatic/amide H refined with riding coordinates:
 C76(H76), C86(H86), C43(H43), C66(H66), C56(H56), C82(H82), C05(H05),
 C74(H74), C45(H45), C84(H84), C42(H42), C44(H44), C03(H03), C72(H72), C62(H62),
  C52(H52), C35(H35), C04(H04), C64(H64), C54(H54), C34(H34), C32(H32),
 C33(H33), C22(H22), C23(H23), C25(H25), C24(H24), C22A(H22G), C23A(H23A),
 C24A(H24A), C25A(H25A), C15(H15), C14(H14), C13(H13), C12(H12), C15A(H15A),
 C14A(H14A), C13A(H13A), C12A(H12A)
6.d Fitted hexagon refined as free rotating group:
 C21(C22,C23,C25,C24,C26), C16(C15,C14,C13,C12,C11)
6.e Idealised Me refined as rotating group:
 C423(H42A,H42B,H42C), C413(H41A,H41B,H41C), C422(H42D,H42E,H42F), C412(H41D,
 H41E,H41F), C223(H22A,H22B,H22C), C222(H22D,H22E,H22F), C213(H21A,H21B,H21C),
 C323(H32A,H32B,H32C), C212(H21D,H21E,H21F), C322(H32D,H32E,H32F), C313(H31A,
 H31B,H31C), C312(H31D,H31E,H31F), C113(H11A,H11B,H11C), C112(H11D,H11E,H11F),
 C122(H12B,H12C,H12D), C123(H12E,H12F,H12G)
;
_shelx_res_checksum              68037
_shelx_hkl_checksum              57762
_olex2_submission_special_instructions 'No special instructions were received'