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_7121894
_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 Fe N5 Si'
_chemical_formula_sum            'C33 H51 Fe N5 Si'
_chemical_formula_weight         601.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-12-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_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                 103.40(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.752(12)
_cell_length_b                   8.725(5)
_cell_length_c                   19.801(10)
_cell_measurement_reflns_used    3213
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.2
_cell_measurement_theta_min      3.2
_cell_volume                     3320(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 13.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9170
              2theta: -15.1669
scan:
    Number of images: 300
               Slice: -105.0000 - 45.0000
         Image width: 0.5000
            Exp time: 13.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9170
              2theta: -15.1669
scan:
    Number of images: 200
               Slice: -105.0000 - -5.0000
         Image width: 0.5000
            Exp time: 13.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9170
              2theta: -15.1669
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.077898
_diffrn_orient_matrix_UB_12      -0.058659
_diffrn_orient_matrix_UB_13      -0.060219
_diffrn_orient_matrix_UB_21      0.023210
_diffrn_orient_matrix_UB_22      0.044494
_diffrn_orient_matrix_UB_23      -0.013302
_diffrn_orient_matrix_UB_31      0.023983
_diffrn_orient_matrix_UB_32      -0.013367
_diffrn_orient_matrix_UB_33      0.044213
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0814
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31563
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.519
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1296
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.934
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7613
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1230
_refine_ls_R_factor_gt           0.0650
_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^)+(0.0040P)^2^+9.9644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1436
_reflns_number_gt                4830
_reflns_number_total             7613
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc03734e2.cif
_cod_data_source_block           m20161211c_pl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7121893--7121897.cif.
;
_cod_database_code               7121894
_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(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(H28A)=Sof(C31')=Sof(H31')=Sof(C32')=Sof(H32D)=Sof(H32E)=Sof(H32F)=
 Sof(C33')=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C16')=Sof(H16C)=Sof(H16D)=
 Sof(C20')=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C19')=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=Sof(C21')=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C29')=Sof(H29D)=
 Sof(H29E)=Sof(H29F)=Sof(C9')=Sof(H9'A)=Sof(H9'B)=Sof(H9'C)=Sof(C13')=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C14')=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15')=
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C11')=Sof(H11D)=Sof(H11E)=Sof(H11F)=
 Sof(C10')=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C30')=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=1-FVAR(1)
 Sof(H28)=Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C32)=Sof(H32A)=Sof(H32B)=
 Sof(H32C)=Sof(C31)=Sof(H31)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C21)=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C19)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=
 Sof(H30B)=Sof(H30C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C14)=Sof(H14A)=
 Sof(H14B)=Sof(H14C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=
 Sof(H11B)=Sof(H11C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C28(H28), C28(H28A), C31(H31), C31'(H31')
4.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C16'(H16C,H16D)
4.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C6(H6), C24(H24), C25(H25), C7(H7), C4(H4), C5(H5), C3(H3)
4.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C21(H21A,H21B,H21C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C15(H15A,
 H15B,H15C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C9(H9A,H9B,H9C),
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C32'(H32D,H32E,H32F), C33'(H33D,H33E,
 H33F), C20'(H20D,H20E,H20F), C19'(H19D,H19E,H19F), C21'(H21D,H21E,H21F),
 C29'(H29D,H29E,H29F), C9'(H9'A,H9'B,H9'C), C13'(H13D,H13E,H13F), C14'(H14D,
 H14E,H14F), C15'(H15D,H15E,H15F), C11'(H11D,H11E,H11F), C10'(H10D,H10E,H10F),
 C30'(H30D,H30E,H30F)
;
_olex2_submission_special_instructions 'No special instructions were received'