Asymmetrically substituted triazenes as poor electron donor ligands in the precursor chemistry of iron(II) for iron-based metallic and intermetallic nanocrystals
Soussi, Khaled; Mishra, Shashank; Jeanneau, Erwann; Millet, Jean-Marc M; Daniele, Stephane; Dalton Trans.  (2017) –; doi:10.1039/C7DT02755A

data_7044130
_publ_section_title
;
 Asymmetrically substituted triazenes as poor electron donor ligands in
 the precursor chemistry of iron(II) for iron-based metallic and
 intermetallic nanocrystals
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02755A
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H44 Fe1 N8'
_chemical_formula_sum            'C18 H44 Fe N8'
_chemical_formula_weight         428.45
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-12
_audit_creation_method           CRYSTALS_ver_14.61
_audit_update_record
;
2017-06-09 deposited with the CCDC.
2017-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6602(3)
_cell_length_b                   8.9362(2)
_cell_length_c                   15.8756(3)
_cell_measurement_reflns_used    10493
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.3970
_cell_measurement_theta_min      4.1090
_cell_volume                     2505.41(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9897
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33283
_diffrn_reflns_theta_full        26.720
_diffrn_reflns_theta_max         29.647
_diffrn_reflns_theta_min         2.859
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.620
_exptl_absorpt_correction_T_max  0.874
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936.000
_exptl_crystal_size_max          0.574
_exptl_crystal_size_mid          0.392
_exptl_crystal_size_min          0.233
_refine_diff_density_max         0.65
_refine_diff_density_min         -0.59
_refine_ls_abs_structure_details 'Flack (1983), 2859 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.32(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9578
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6216
_refine_ls_number_restraints     521
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.0004046
_refine_ls_shift/su_mean         0.0000227
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.207E+04 0.316E+04 0.174E+04 624. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1271
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1271
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              11
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              -21
_reflns_number_gt                5274
_reflns_number_total             6225
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.56
_oxford_diffrn_Wilson_scale      0.04
_oxford_refine_ls_r_factor_ref   0.0688
_oxford_refine_ls_scale          6.41(13)
_oxford_reflns_number_all        6216
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'SIR2014 run in space group P n a 21'
_cod_data_source_file            c7dt02755a1.cif
_cod_data_source_block           'global_CCDC3'
_cod_original_sg_symbol_H-M      'P n a 21 '
_cod_original_formula_sum        'C18 H44 Fe1 N8'
_cod_database_code               7044130
_oxdiff_exptl_absorpt_empirical_full_min 0.700
_oxdiff_exptl_absorpt_empirical_full_max 1.432
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;