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_7132108
_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 N4.502 Si4'
_chemical_formula_sum            'C16 H45 Fe N4.5 Si4'
_chemical_formula_weight         468.77
_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             2023-07-24
_audit_creation_method
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Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
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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                 100.264(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.883(4)
_cell_length_b                   16.016(6)
_cell_length_c                   20.510(8)
_cell_measurement_reflns_used    3565
_cell_measurement_temperature    80.00
_cell_measurement_theta_max      21.546
_cell_measurement_theta_min      2.391
_cell_volume                     2871(2)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      80.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.1210
_diffrn_reflns_av_unetI/netI     0.1433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21934
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.049
_diffrn_reflns_theta_min         2.369
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1436 before and 0.0631 after correction.
The Ratio of minimum to maximum transmission is 0.8018.
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    1.084
_exptl_crystal_description       plate
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         5648
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0694
_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^)+(0.0480P)^2^+5.2460P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1807
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3398
_reflns_number_total             5648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03765g2.cif
_cod_data_source_block           1b
_cod_original_formula_sum        'C16 H45 Fe N4.50 Si4'
_cod_database_code               7132108
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.933
_olex2_refinement_description
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1. Restrained distances
 Si2-C3
 1.85 with sigma of 0.02
 Si2-C16
 1.85 with sigma of 0.02
 Fe1-N5 \\sim Fe1-N5A
 with sigma of 0.02
 Si05-N5 \\sim Si05-N5A
 with sigma of 0.02
 N5-Si1 \\sim N5A-Si1
 with sigma of 0.02
 Si04-N5 \\sim Si04-N5A
 with sigma of 0.02
 N5-Si2 \\sim N5A-Si2
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5A) \\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: Si04(0.85) Si05(0.85) N5(0.85) C00I(0.85) H00S(0.85) H00T(0.85)
 H00U(0.85) H00Y(0.85) H(0.85) HA(0.85) HB(0.15) HC(0.15) HD(0.15) C00N(0.85)
 H1(0.85) HI(0.85) HJ(0.85) H2(0.85) HK(0.85) HL(0.85) HM(0.15) HN(0.15)
 HO(0.15) C00P(0.85) H3(0.85) HP(0.85) HQ(0.85) C00Q(0.85) H4(0.85) HR(0.85)
 HS(0.85) Si1(0.15) C4(0.15) H4A(0.15) H4B(0.15) H4C(0.15) Si2(0.15) C3(0.15)
 H3A(0.15) H3B(0.15) H3C(0.15) C7(0.15) H7A(0.15) H7B(0.15) H7C(0.15) C16(0.15)
 H16A(0.15) H16B(0.15) H16C(0.15) N5A(0.15)
4.a Idealised Me refined as rotating group:
 C00B(H00A,H00B,H00C), C00C(H00D,H00E,H00F), C00E(H00G,H00H,H00I), C00F(H00J,
 H00K,H00L), C00G(H00M,H00N,H00O), C00H(H00P,H00Q,H00R), C00I(H00S,H00T,H00U),
 C00J(H00V,H00W,H00X), C00K(H00Y,H,HA), C00K(HB,HC,HD), C00L(H00Z,HE,HF),
 C00M(H00,HG,HH), C00N(H1,HI,HJ), C00O(H2,HK,HL), C00O(HM,HN,HO), C00P(H3,HP,
 HQ), C00Q(H4,HR,HS), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C), C7(H7A,H7B,H7C),
 C16(H16A,H16B,H16C)
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_shelx_res_checksum              15330
_olex2_submission_special_instructions 'No special instructions were received'