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_4318658
_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 H16 N4 Cl2 Fe Br2'
_chemical_formula_sum            'C18 H16 Br2 Cl2 Fe N4'
_chemical_formula_weight         574.93
_chemical_name_systematic        ' ?'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 99.201(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4198(5)
_cell_length_b                   10.9214(8)
_cell_length_c                   11.3218(7)
_cell_measurement_reflns_used    7495
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      1.4
_cell_volume                     1027.71(12)
_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, 20 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times.
Detector to crystal distance 25 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  0.074
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7495
_diffrn_reflns_theta_max         26.38
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.859
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.86
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.300
_refine_ls_abs_structure_Flack   0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.214
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     243
_refine_ls_number_reflns         1511
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.061
_refine_ls_R_factor_gt           0.034
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0009 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.045
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                1511
_reflns_number_total             2220
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            ic011104t_s2.cif
_cod_data_source_block           L3Fe(II)Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0009
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^) + 0.0009 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1027.7(2)
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_original_formula_sum        'C18 H16 N4 Cl2 Fe Br2'
_cod_database_code               4318658
_cod_database_fobs_code          4318658