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_7121895
_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         'C33 H51 Br2 Fe N3 Si, C7 H8'
_chemical_formula_sum            'C40 H59 Br2 Fe N3 Si'
_chemical_formula_weight         825.66
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-03-21 deposited with the CCDC.
2018-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.503(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.408(4)
_cell_length_b                   19.199(5)
_cell_length_c                   17.680(6)
_cell_measurement_reflns_used    1683
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      25.4
_cell_measurement_theta_min      3.0
_cell_volume                     4176(2)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_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      386.3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Xtalab P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2476
_diffrn_reflns_av_unetI/netI     0.2809
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44783
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         3.016
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9559
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.3038
_refine_ls_R_factor_gt           0.1076
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+16.4499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1724
_refine_ls_wR_factor_ref         0.2438
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3310
_reflns_number_total             9559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc03734e2.cif
_cod_data_source_block           sa
_cod_depositor_comments
'Adding full bibliography for 7121893--7121897.cif.'
_cod_database_code               7121895
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.679
_shelx_estimated_absorpt_t_min   0.628
_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. Restrained distances
 C34-C35 = C34'-C35'
 1.5 with sigma of 0.01
 C34-C36 \\sim C34-C40 \\sim C34'-C36' \\sim C34'-C40'
 with sigma of 0.01
3. Restrained planarity
 C34, C35, C36, C37, C38, C39, C40
 with sigma of 0.01
 C34', C35', C36', C37', C38', C39', C40'
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq,
Uanis(C34') \\sim Ueq, Uanis(C35') \\sim Ueq, Uanis(C36') \\sim Ueq,
Uanis(C37') \\sim Ueq, Uanis(C38') \\sim Ueq, Uanis(C39') \\sim Ueq,
Uanis(C40') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C34')=Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35')=Sof(C36')=Sof(H36')=
 Sof(C37')=Sof(H37')=Sof(C38')=Sof(H38')=Sof(C39')=Sof(H39')=Sof(C40')=
 Sof(H40')=1-FVAR(1)
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(C36)=Sof(H36)=Sof(C37)=
 Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C28(H28), C31(H31)
6.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
6.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C24(H24), C25(H25),
 C26(H26), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C36'(H36'),
 C37'(H37'), C38'(H38'), C39'(H39'), C40'(H40')
6.d Fitted hexagon refined as free rotating group:
 C35(C36,C37,C38,C39,C40), C35'(C36',C37',C38',C39',C40')
6.e Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,
 H8B,H8C), C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,
 H21B,H21C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C),
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C34'(H34D,H34E,H34F)
;
_shelx_res_checksum              24312
_olex2_submission_special_instructions 'No special instructions were received'