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_7044127
_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         'C20 H48 Fe1 N8'
_chemical_formula_sum            'C20 H48 Fe N8'
_chemical_formula_weight         456.50
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-26
_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                 92.280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8650(10)
_cell_length_b                   16.262(2)
_cell_length_c                   16.402(2)
_cell_measurement_reflns_used    6017
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.3580
_cell_measurement_theta_min      3.6890
_cell_volume                     2629.2(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.912
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18348
_diffrn_reflns_theta_full        25.138
_diffrn_reflns_theta_max         29.574
_diffrn_reflns_theta_min         2.796
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  0.823
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.384
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.74
_refine_ls_abs_structure_details 'Flack (1983), 1942 Friedel-pairs'
_refine_ls_extinction_coef       37(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9633
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.0005898
_refine_ls_shift/su_mean         0.0000405
_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: 
 0.165E+04 0.243E+04 0.135E+04 427. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1013
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1013
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                2930
_reflns_number_total             3370
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0572
_oxford_refine_ls_scale          3.72(5)
_oxford_reflns_number_all        3366
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'kso-a-011 in C 1 2/c 1'
_cod_data_source_file            c7dt02755a1.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_original_formula_sum        'C20 H48 Fe1 N8'
_cod_database_code               7044127