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_7132113
_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         'C22 H63 Fe2 K N4 Si6'
_chemical_formula_sum            'C22 H63 Fe2 K N4 Si6'
_chemical_formula_weight         703.10
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-28
_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                 93.938(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2649(4)
_cell_length_b                   14.9686(6)
_cell_length_c                   27.6440(11)
_cell_measurement_reflns_used    9928
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.745
_cell_measurement_theta_min      2.590
_cell_volume                     3824.7(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 1.000
_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  0.0414
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            95490
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.765
_diffrn_reflns_theta_min         2.203
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.073
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6773
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1192 before and 0.0539 after correction.
The Ratio of minimum to maximum transmission is 0.9086.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'dark orange'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       plate
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.312
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0284
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+3.4233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7396
_reflns_number_total             8137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03765g2.cif
_cod_data_source_block           3
_cod_database_code               7132113
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.731
_olex2_refinement_description
;
1.a Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C11(H11A,H11B,
 H11C), C19(H19A,H19B,H19C), C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C14(H14A,
 H14B,H14C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C8(H8A,H8B,H8C), C2(H2A,
 H2B,H2C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C4(H4A,H4B,H4C), C3(H3A,H3B,H3C)
;
_shelx_res_checksum              81218
_olex2_submission_special_instructions 'No special instructions were received'