Trigonal Bipyramidal Geometry and Tridentate Coordination Mode of the Tripod in FeCl2 Complexes with Tris(2-pyridylmethyl)amine Derivatives Bis-α-Substituted with Bulky Groups. Structures and Spectroscopic Comparative Studies
Dominique Mandon; Ahmed Machkour; Sandrine Goetz; Richard Welter; Inorganic Chemistry 41 (2002) 5364–5372; doi:10.1021/ic011104t

data_4318657
_publ_section_title
;
 Trigonal Bipyramidal Geometry and Tridentate Coordination Mode of the
 Tripod in FeCl2 Complexes with Tris(2-pyridylmethyl)amine Derivatives
 Bis-\a-Substituted with Bulky Groups. Structures and Spectroscopic
 Comparative Studies
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5364
_journal_page_last               5372
_journal_paper_doi               10.1021/ic011104t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         'C68 H66 Cl4 Fe2 N11 O'
_chemical_formula_sum            'C68 H66 Cl4 Fe2 N11 O'
_chemical_formula_weight         1306.86
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                113.786(6)
_cell_angle_beta                 94.924(6)
_cell_angle_gamma                91.108(6)
_cell_formula_units_Z            1
_cell_length_a                   9.1141(3)
_cell_length_b                   12.6745(7)
_cell_length_c                   15.6581(7)
_cell_measurement_reflns_used    10310
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.4
_cell_volume                     1646.13(15)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      173
_diffrn_measurement_details
;
  10310 reflections were collected using program Collect
 ("Collect" Data collection software, Nonius B.V., 1998)
 The conditions were as follow : crystal to detector distance =  36. mm.
 Scan angle =  2.0 deg 1 scans of   89 sec per frame.
 Data collection was divided into  3 set(s)
 with the following starting angles and number of frames :

 Set 1 Theta =    6.40 Omega =    0.00 Kappa =    0.00   91 frames
 Set 2 Theta =   -5.40 Kappa =  139.00 Phi   =    0.00   17 frames
 Set 3 Theta =   -6.40 Kappa = -172.00 Phi   =    0.00   19 frames
 Friedel pairs were averaged. Internal R = 0.04
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10310
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             679
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.780
_refine_ls_goodness_of_fit_ref   1.202
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     382
_refine_ls_number_reflns         4006
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.117
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.158
_refine_ls_wR_factor_ref         0.075
_reflns_number_gt                4006
_reflns_number_total             7457
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic011104t_s1.cif
_cod_data_source_block           L4Fe(II)Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0064
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0064 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1646.1(3)
_cod_database_code               4318657