Lattice-Dictated Conformers in Bis(pyrazolyl)pyridine-Based Iron(II) Complexes: Mössbauer, NMR, and Magnetic Studies
P. Manikandan; K. Padmakumar; K. R. Justin Thomas; B. Varghese; P. T. Manoharan; Inorganic Chemistry 40 (2001) 6930–6939; doi:10.1021/ic010655g

data_4320776
_publ_section_title
;
 Lattice-Dictated Conformers in Bis(pyrazolyl)pyridine-Based Iron(II)
 Complexes: M\"ossbauer, NMR, and Magnetic Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6930
_journal_page_last               6939
_journal_paper_doi               10.1021/ic010655g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C34 H42 F12 Fe N10 P2'
_chemical_formula_weight         936.57
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   12.6452(10)
_cell_length_b                   15.361(3)
_cell_length_c                   42.412(5)
_cell_measurement_temperature    293(2)
_cell_volume                     8238(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.452
_diffrn_measured_fraction_theta_max 0.452
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3635
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.538
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3840
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.00031(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.206
_refine_ls_shift/su_mean         0.044
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+32.5828P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                2446
_reflns_number_total             3615
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010655g_2.cif
_cod_data_source_block           '[FeL2][PF6]2'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+32.5828P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+32.5828P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        8239(2)
_cod_database_code               4320776