An arene-tethered silylene ligand enabling reversible dinitrogen binding to iron and catalytic silylation.
Bai, Yunping; Zhang, Jianying; Cui, Chunming; Chemical communications (Cambridge, England) 54 (2018) 8124–8127; doi:10.1039/c8cc03734e

data_7121896
_publ_section_title
;
 An arene-tethered silylene ligand enabling reversible dinitrogen binding
 to iron and catalytic silylation.
;
_journal_issue                   58
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8124
_journal_page_last               8127
_journal_paper_doi               10.1039/c8cc03734e
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C66 H102 Fe N6 Si2'
_chemical_formula_sum            'C66 H102 Fe N6 Si2'
_chemical_formula_weight         1091.57
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-01-25
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-05-28 deposited with the CCDC.
2018-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                86.591(12)
_cell_angle_beta                 82.254(10)
_cell_angle_gamma                87.814(12)
_cell_formula_units_Z            2
_cell_length_a                   10.351(3)
_cell_length_b                   12.058(3)
_cell_length_c                   26.098(6)
_cell_measurement_reflns_used    5068
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      3.2
_cell_volume                     3220.4(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1037
_diffrn_reflns_av_unetI/netI     0.1122
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            27980
_diffrn_reflns_theta_full        24.50
_diffrn_reflns_theta_max         24.50
_diffrn_reflns_theta_min         3.16
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.314
_exptl_absorpt_correction_T_max  0.9399
_exptl_absorpt_correction_T_min  0.9399
_exptl_crystal_density_diffrn    1.126
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1188
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.291
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10246
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1263
_refine_ls_R_factor_gt           0.0855
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1741P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2233
_refine_ls_wR_factor_ref         0.2678
_reflns_number_gt                6435
_reflns_number_total             10246
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc03734e2.cif
_cod_data_source_block           m20170705a_sqd
_cod_depositor_comments
'Adding full bibliography for 7121893--7121897.cif.'
_cod_original_cell_volume        3220.5(13)
_cod_database_code               7121896
_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. Uiso/Uaniso restraints and constraints
Uanis(C022) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00I) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=
 Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(1)
 Sof(C2AA)=Sof(H2AB)=Sof(H2AC)=Sof(H2AD)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=
 Sof(C3AA)=Sof(H3AB)=Sof(H3AC)=Sof(H3AD)=FVAR(1)
 Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=Sof(C6)=
 Sof(H6A)=Sof(H6B)=Sof(H6C)=1-FVAR(2)
 Sof(C0AA)=Sof(H0AB)=Sof(H0AC)=Sof(H0AD)=Sof(C1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(H1AD)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(2)
4.a Ternary CH refined with riding coordinates:
 C00I(H00I), C00Y(H00Y), C014(H014), C01F(H01X)
4.b Secondary CH2 refined with riding coordinates:
 C00F(H00A,H00B), C00M(H00C,H00D)
4.c Aromatic/amide H refined with riding coordinates:
 C00J(H00J), C00N(H00N), C00O(H00O), C00P(H00P), C00U(H00U), C016(H016),
 C01B(H01P), C01D(H01T), C01J(H01), C01K(H0AA), C01M(H2AA), C01N(H3AA),
 C01Q(H6AA), C01R(H7AA), C01W(H2BA), C022(H022)
4.d Idealised Me refined as rotating group:
 C00R(H00E,H00F,H00G), C00T(H00H,H00K,H00L), C00X(H00M,H00Q,H00R), C010(H01A,
 H01B,H01C), C011(H01D,H01E,H01F), C017(H01G,H01H,H01I), C019(H01J,H01K,H01L),
 C01A(H01M,H01N,H01O), C01C(H01Q,H01R,H01S), C01E(H01U,H01V,H01W), C01G(H01Y,H,
 HA), C01I(H01Z,HB,HC), C01L(H1AA,HD,HE), C01O(H4AA,HF,HG), C01P(H5AA,HH,HI),
 C01S(H8AA,HJ,HK), C01T(H9AA,HL,HM), C01U(H0BA,HN,HO), C01V(H1BA,HP,HQ),
 C026(H02A,H02B,H02C), C2AA(H2AB,H2AC,H2AD), C1(H1A,H1B,H1C), C3AA(H3AB,H3AC,
 H3AD), C0AA(H0AB,H0AC,H0AD), C1AA(H1AB,H1AC,H1AD), C5(H5A,H5B,H5C), C4(H4A,H4B,
 H4C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C),
 C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'