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_4123803
_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         'C54 H75 Fe2 N4 P4 S Si2, C16 H32 Na O8'
_chemical_formula_sum            'C70 H107 Fe2 N4 Na O8 P4 S Si2'
_chemical_formula_weight         1479.40
_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             2015-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                72.636(2)
_cell_angle_beta                 73.491(3)
_cell_angle_gamma                77.740(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3999(6)
_cell_length_b                   15.4526(7)
_cell_length_c                   21.3794(9)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.95
_cell_measurement_theta_min      2.25
_cell_volume                     4011.4(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0586
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            274074
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.597
_diffrn_reflns_theta_min         1.971
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_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    1.225
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         24597
_refine_ls_number_restraints     1146
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0325
_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^)+(0.0415P)^2^+1.1938P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0827
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19792
_reflns_number_total             24597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04738_si_002.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 4123801--4123807.cif.'
_cod_database_code               4123803
_shelxl_version_number           2014/6
_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
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(C7C1) \\sim Ueq, Uanis(C3C1) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C4C1) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C3C1) = Uanis(C4C2)
Uanis(C7C1) = Uanis(C8C2)
Uanis(C4C1) = Uanis(O2C2)
4. Same fragment restrains
{C1C2, C2C2, O1C2, C3C2, C4C2, O2C2, C5C2, C6C2, O3C2, C7C2, C8C2, O4C2} sigma
for 1-2: 0.02, 1-3: 0.04
{C3C3, C4C3, O2C3, C5C3, C6C3, O3C3, C7C3, C8C3, O4C3, C1C3, C2C3, O1C3} sigma
for 1-2: 0.02, 1-3: 0.04
as
{C1C1, C2C1, O1C1, C3C1, C4C1, O2C1, C5C1, C6C1, O3C1, C7C1, C8C1, O4C1}
5. Others
 Sof(C1C1)=Sof(H1CE)=Sof(H1CF)=Sof(C2C1)=Sof(H2CE)=Sof(H2CF)=Sof(O1C1)=
 Sof(C3C1)=Sof(H3CE)=Sof(H3CF)=Sof(C4C1)=Sof(H4CE)=Sof(H4CF)=Sof(O2C1)=
 Sof(C5C1)=Sof(H5CE)=Sof(H5CF)=Sof(C6C1)=Sof(H6CE)=Sof(H6CF)=Sof(O3C1)=
 Sof(C7C1)=Sof(H7CE)=Sof(H7CF)=Sof(C8C1)=Sof(H8CE)=Sof(H8CF)=Sof(O4C1)=1-FVAR(1)
 Sof(C1C2)=Sof(H1CC)=Sof(H1CD)=Sof(C2C2)=Sof(H2CC)=Sof(H2CD)=Sof(O1C2)=
 Sof(C3C2)=Sof(H3CC)=Sof(H3CD)=Sof(C4C2)=Sof(H4CC)=Sof(H4CD)=Sof(O2C2)=
 Sof(C5C2)=Sof(H5CC)=Sof(H5CD)=Sof(C6C2)=Sof(H6CC)=Sof(H6CD)=Sof(O3C2)=
 Sof(C7C2)=Sof(H7CC)=Sof(H7CD)=Sof(C8C2)=Sof(H8CC)=Sof(H8CD)=Sof(O4C2)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C00Z(H00Z), C012(H012), C015(H015), C016(H016), C01E(H01E), C01G(H01G),
 C01J(H01J), C01W(H2AA)
6.b Secondary CH2 refined with riding coordinates:
 C3C3(H3CA,H3CB), C4C3(H4CA,H4CB), C5C3(H5CA,H5CB), C6C3(H6CA,H6CB), C7C3(H7CA,
 H7CB), C8C3(H8CA,H8CB), C1C3(H1CA,H1CB), C2C3(H2CA,H2CB), C1C2(H1CC,H1CD),
 C2C2(H2CC,H2CD), C3C2(H3CC,H3CD), C4C2(H4CC,H4CD), C5C2(H5CC,H5CD), C6C2(H6CC,
 H6CD), C7C2(H7CC,H7CD), C8C2(H8CC,H8CD), C1C1(H1CE,H1CF), C2C1(H2CE,H2CF),
 C3C1(H3CE,H3CF), C4C1(H4CE,H4CF), C5C1(H5CE,H5CF), C6C1(H6CE,H6CF), C7C1(H7CE,
 H7CF), C8C1(H8CE,H8CF)
6.c Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00S(H00S), C00V(H00V), C00W(H00W), C00X(H00X), C00Y(H00Y),
 C014(H014), C019(H019), C01A(H01A), C01B(H01B), C01C(H01C), C01D(H01D),
 C01F(H01F), C01H(H01H), C01I(H01I), C01M(H01Q), C01N(H01R), C01O(H01S),
 C01Q(H01W)
6.d Idealised Me refined as rotating group:
 C01K(H01K,H01L,H01M), C01L(H01N,H01O,H01P), C01P(H01T,H01U,H01V), C01R(H01X,
 H01Y,H), C01S(H01Z,HA,HB), C01T(H01,HC,HD), C01U(H0AA,HE,HF), C01V(H1AA,HG,HH),
  C01X(H3AA,HI,HJ), C01Y(H4AA,HK,HL), C01Z(H5AA,HM,HN), C020(H02A,H02B,H02C),
 C021(H02D,H02E,H02F), C022(H02G,H02H,H02I), C025(H02J,H02K,H02L), C02A(H02M,
 H02N,H02O)
;
_shelx_res_checksum              15845
_shelx_hkl_checksum              53342
_olex2_submission_special_instructions 'No special instructions were received'