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_7132110
_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 N3 Si4'
_chemical_formula_sum            'C16 H45 Fe N3 Si4'
_chemical_formula_weight         447.76
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-03-31
_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                 106.253(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3458(4)
_cell_length_b                   19.5220(7)
_cell_length_c                   15.2414(7)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      29.964
_cell_measurement_theta_min      2.498
_cell_volume                     2669.64(19)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.925
_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  0.0441
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18947
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.035
_diffrn_reflns_theta_min         2.086
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.749
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0735 before and 0.0501 after correction.
The Ratio of minimum to maximum transmission is 0.9216.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.183
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         7221
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0578P)^2^+0.1620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1139
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5572
_reflns_number_total             7221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03765g2.cif
_cod_data_source_block           2
_cod_database_code               7132110
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.833
_olex2_refinement_description
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1. Restrained distances
 Fe1-N008 \\sim Fe1-N3
 with sigma of 0.02
 Si4-C12 \\sim Si4-C00P
 with sigma of 0.02
 N008-C13 \\sim N3-C13
 with sigma of 0.02
 Si4-N008 \\sim Si4-N3
 with sigma of 0.04
 N008-C12 \\sim N3-C00P
 with sigma of 0.02
 C13-C12 \\sim C13-C00P
 with sigma of 0.04
 Fe1-C12 \\sim Fe1-C00P
 with sigma of 0.04
2. Others
 Sof(C00P)=Sof(H00A)=Sof(H00B)=Sof(N3)=Sof(H3)=1-FVAR(1)
 Sof(N008)=Sof(H008)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 N008(H008), N3(H3)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C00P(H00A,H00B)
3.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C),
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C15(H15A,
 H15B,H15C), C14(H14A,H14B,H14C), C11(H11A,H11B,H11C), C7(H7A,H7B,H7C), C2(H2A,
 H2B,H2C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              39145
_olex2_submission_special_instructions 'No special instructions were received'