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_7044129
_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         'C22 H52 Fe N8'
_chemical_formula_sum            'C22 H52 Fe N8'
_chemical_formula_weight         484.57
_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             2016-01-19
_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                 98.1363(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6188(2)
_cell_length_b                   16.6011(2)
_cell_length_c                   18.2778(3)
_cell_measurement_reflns_used    8382
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.6580
_cell_measurement_theta_min      3.9050
_cell_volume                     2889.27(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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 0.982
_diffrn_measured_fraction_theta_max 0.913
_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  0.027
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19548
_diffrn_reflns_theta_full        25.053
_diffrn_reflns_theta_max         29.132
_diffrn_reflns_theta_min         3.129
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.835
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            'dark brown'
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.317
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.45
_refine_ls_abs_structure_details 'Flack (1983), 3184 Friedel-pairs'
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9754
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     141
_refine_ls_number_reflns         3552
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.0011502
_refine_ls_shift/su_mean         0.0000408
_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: 
 582. 842. 415. 104. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0652
_refine_ls_wR_factor_gt          0.0624
_refine_ls_wR_factor_ref         0.0652
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                3164
_reflns_number_total             3556
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.55
_oxford_diffrn_Wilson_scale      0.85
_oxford_refine_ls_r_factor_ref   0.0445
_oxford_refine_ls_scale          2.822(14)
_oxford_reflns_number_all        3552
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'kso_a_046 in C 1 c 1'
_cod_data_source_file            c7dt02755a1.cif
_cod_data_source_block           'global_CCDC2'
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_database_code               7044129
_oxdiff_exptl_absorpt_empirical_full_min 0.810
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;