A low-coordinate iron organoazide complex.
Gonzalez, Andres; Demeshko, Serhiy; Meyer, Franc; Werncke, C. Gunnar; Chemical communications (Cambridge, England)  (2023) –; doi:10.1039/d3cc03765g

data_7132112
_publ_section_title
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 A low-coordinate iron organoazide complex.
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_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/d3cc03765g
_journal_year                    2023
_chemical_formula_moiety         'C16 H45 Fe N4.307 Si4'
_chemical_formula_sum            'C16 H45 Fe N4.31 Si4'
_chemical_formula_weight         466.08
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-30
_audit_creation_method
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FinalCif V113 by Daniel Kratzert, Freiburg 2023,
https://dkratzert.de/finalcif.html
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_audit_update_record
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2023-07-24 deposited with the CCDC.	2023-08-30 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 100.299(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8341(17)
_cell_length_b                   15.935(3)
_cell_length_c                   20.441(4)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    80.00
_cell_measurement_theta_max      25.338
_cell_measurement_theta_min      2.381
_cell_volume                     2831.1(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      80.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1714
_diffrn_reflns_av_unetI/netI     0.0960
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58649
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.381
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5801
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1574 before and 0.0872 after correction.
The Ratio of minimum to maximum transmission is 0.7783.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       plate
_exptl_crystal_F_000             1013
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.034
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5558
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1301
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0733P)^2^+10.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2032
_refine_ls_wR_factor_ref         0.2175
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3653
_reflns_number_total             5558
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03765g2.cif
_cod_data_source_block           1c
_cod_original_cell_volume        2831.2(9)
_cod_database_code               7132112
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.976
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
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1. Restrained distances
 Si4-C11
 1.85 with sigma of 0.02
 Si3-C15
 1.85 with sigma of 0.02
 C11-Si3 \\sim C15-Si3
 with sigma of 0.02
 Si4-C11 \\sim Si4-C15
 with sigma of 0.02
 Si5-N6 \\sim Si5-N5
 with sigma of 0.02
 Si4-N6 \\sim Si4-N5
 with sigma of 0.02
 N6-Si3 \\sim N5-Si3
 with sigma of 0.02
 Fe1-N6 \\sim Fe1-N5
 with sigma of 0.02
 N6-Si6 \\sim N5-Si6
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(Si3) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.1
Uanis(C19) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(N2)=Sof(N3)=FVAR(1)
 Fixed Sof: Si5(0.8) Si4(0.8) N6(0.8) C11(0.8) H11A(0.8) H11B(0.8) H11C(0.8)
 C16(0.8) H16A(0.8) H16B(0.8) H16C(0.8) H12A(0.8) H12B(0.8) H12C(0.8) H12D(0.2)
 H12E(0.2) H12F(0.2) H18A(0.8) H18B(0.8) H18C(0.8) H18D(0.2) H18E(0.2)
 H18F(0.2) C20(0.8) H20A(0.8) H20B(0.8) H20C(0.8) C13(0.8) H13A(0.8) H13B(0.8)
 H13C(0.8) Si3(0.2) C14(0.2) H14A(0.2) H14B(0.2) H14C(0.2) Si6(0.2) C19(0.2)
 H19A(0.2) H19B(0.2) H19C(0.2) C17(0.2) H17A(0.2) H17B(0.2) H17C(0.2) C15(0.2)
 H15A(0.2) H15B(0.2) H15C(0.2) N5(0.2)
4.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C8(H8A,H8B,H8C), C3(H3A,
 H3B,H3C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C2(H2A,H2B,H2C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C), C12(H12D,
 H12E,H12F), C18(H18A,H18B,H18C), C18(H18D,H18E,H18F), C20(H20A,H20B,H20C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C17(H17A,H17B,
 H17C), C15(H15A,H15B,H15C)
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_shelx_res_checksum              86831
_olex2_submission_special_instructions 'No special instructions were received'