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_4318660
_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
;
_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         'C18 H18 N4 Cl2 Fe'
_chemical_formula_sum            'C18 H18 Cl2 Fe N4'
_chemical_formula_weight         417.12
_chemical_name_systematic        ' ?'
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   18.516(1)
_cell_length_b                   16.157(1)
_cell_length_c                   25.450(1)
_cell_measurement_reflns_used    16523
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.4
_cell_volume                     7613.7(7)
_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
;
180 frames, 30 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times.
Detector to crystal distance 35 mm.
;
_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  0.060
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            16523
_diffrn_reflns_theta_max         26.35
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.46
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.393
_refine_diff_density_min         -0.192
_refine_ls_abs_structure_details ' ?'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   *****
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     451
_refine_ls_number_reflns         3842
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.131
_refine_ls_R_factor_gt           0.041
_refine_ls_shift/esd_mean        0.004
_refine_ls_shift/su_max          0.025
_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         0.806
_refine_ls_wR_factor_ref         0.058
_reflns_number_gt                3842
_reflns_number_total             7309
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic011104t_s4.cif
_cod_data_source_block           L1Fe(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        7613(1)
_cod_original_formula_sum        'C18 H18 N4 Cl2 Fe'
_cod_database_code               4318660
_cod_database_fobs_code          4318660