Synthesis of Silyl Iron Dinitrogen Complexes for Activation of Dihydrogen and Catalytic Silylation of Dinitrogen
Chang, Guoliang; Zhang, Peng; Yang, Wenjing; Dong, Yanhong; Xie, Shangqing; Sun, Hongjian; Li, Xiaoyan; Fuhr, Olaf; Fenske, Dieter; Dalton Transactions  (2021) –; doi:10.1039/D1DT02832D

data_7708677
_publ_section_title
;
 Synthesis of Silyl Iron Dinitrogen Complexes for Activation of Dihydrogen
 and Catalytic Silylation of Dinitrogen
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02832D
_journal_year                    2021
_chemical_formula_moiety         'C28 H49 Fe N2 P3 Si'
_chemical_formula_sum            'C28 H49 Fe N2 P3 Si'
_chemical_formula_weight         590.54
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-07-10 deposited with the CCDC.	2021-11-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.988(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.4753(4)
_cell_length_b                   17.1665(4)
_cell_length_c                   13.9116(4)
_cell_measurement_reflns_used    21386
_cell_measurement_temperature    153.15
_cell_measurement_theta_max      63.31
_cell_measurement_theta_min      4.04
_cell_volume                     3093.61(15)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            DECTRIS
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       '4-circle goniometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15684
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        62.913
_diffrn_reflns_theta_max         62.913
_diffrn_reflns_theta_min         4.191
_diffrn_source                   'Cu Genix 3D'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_target            Cu
_diffrn_source_type              'microfocus sealed X-ray tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.884
_exptl_absorpt_correction_T_max  0.4917
_exptl_absorpt_correction_T_min  0.2970
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE Xred and LANA'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       cube
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.752
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         4868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0606P)^2^+4.7089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1195
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4416
_reflns_number_total             4868
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02832d2.cif
_cod_data_source_block           sun44b
_cod_original_cell_volume        3093.60(15)
_cod_database_code               7708677
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C8(H10), C11(H20), C20(H7), C23(H2)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H23), C5(H14), C6(H11), C7(H21), C16(H8), C17(H17), C18(H4), C19(H12)
2.c Idealised Me refined as rotating group:
 C1(H0AA,H0AB,H0AC), C9(H26A,H26B,H26C), C10(H24A,H24B,H24C), C12(H15A,H15B,
 H15C), C13(H25A,H25B,H25C), C21(H6A,H6B,H6C), C22(H19A,H19B,H19C), C24(H16A,
 H16B,H16C), C25(H22A,H22B,H22C), C26(H27A,H27B,H27C), C27(H29A,H29B,H29C),
 C28(H31A,H31B,H31C)
;
_shelx_res_checksum              61426
_shelx_hkl_checksum              98676
_olex2_submission_special_instructions 'No special instructions were received'