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_7121897
_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         'C45 H87 Fe N5 Si5'
_chemical_formula_sum            'C45 H87 Fe N5 Si5'
_chemical_formula_weight         894.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-03-21 deposited with the CCDC.
2018-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.912(4)
_cell_length_b                   16.921(3)
_cell_length_c                   30.492(6)
_cell_measurement_reflns_used    14770
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.0472
_cell_measurement_theta_min      1.6528
_cell_volume                     10790(4)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1533
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            106532
_diffrn_reflns_theta_full        26.08
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         1.34
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.423
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3904
_refine_diff_density_max         0.832
_refine_diff_density_min         -1.087
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.0054(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         10660
_refine_ls_number_restraints     336
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1166
_refine_ls_R_factor_gt           0.0845
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1164P)^2^+12.2304P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2299
_reflns_number_gt                7965
_reflns_number_total             10660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc03734e2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 7121893--7121897.cif.'
_cod_database_code               7121897
_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
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C28(H28), C31(H31)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
3.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C24(H24), C25(H25), C11(H11), C13(H13), C12(H12), C14(H14), C15(H15)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C34(H34A,H34B,H34C), C9(H9A,H9B,H9C), C44(H44A,H44B,
 H44C), C3(H3A,H3B,H3C), C8(H8A,H8B,H8C), C45(H45A,H45B,H45C), C42(H42A,H42B,
 H42C), C29(H29A,H29B,H29C), C21(H21A,H21B,H21C), C32(H32A,H32B,H32C), C43(H43A,
 H43B,H43C), C19(H19A,H19B,H19C), C39(H39A,H39B,H39C), C30(H30A,H30B,H30C),
 C4(H4A,H4B,H4C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C41(H41A,H41B,H41C),
  C33(H33A,H33B,H33C), C7(H7A,H7B,H7C), C40(H40A,H40B,H40C), C5(H5A,H5B,H5C),
 C36(H36A,H36B,H36C), C38(H38A,H38B,H38C)
;
_olex2_submission_special_instructions 'No special instructions were received'