Fluorinated mixed valence Fe(II)-Fe(III) phosphites with channels templated by linear tetramine chains. Structural and magnetic implications of partial replacement of Fe(II) by Co(II)
Orive Gomez de Segura, Joseba; Fernández de Luis, Roberto; Rodriguez Fernandez, J.; Legarra, Estibaliz; Plazaola, Fernando; Arriortua, María Isabel; CrystEngComm  (2014) –; doi:10.1039/c4ce00264d

data_7215775
_publ_section_title
;
 Fluorinated mixed valence Fe(II)-Fe(III) phosphites with channels
 templated by linear tetramine chains. Structural and magnetic
 implications of partial replacement of Fe(II) by Co(II)
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/c4ce00264d
_journal_year                    2014
_chemical_formula_sum            'C3.5 H19.7 F4 Fe4 N2 O14.43 P4'
_chemical_formula_weight         744.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-12-18T16:04:12-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 116.983(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6808(4)
_cell_length_b                   12.6340(2)
_cell_length_c                   12.7830(3)
_cell_measurement_reflns_used    9552
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1663
_cell_measurement_theta_min      1.6086
_cell_volume                     1968.94(11)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.2439
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0291564
_diffrn_orient_matrix_UB_12      0.0019422
_diffrn_orient_matrix_UB_13      0.0621305
_diffrn_orient_matrix_UB_21      0.0501257
_diffrn_orient_matrix_UB_22      -0.0061583
_diffrn_orient_matrix_UB_23      -0.0031591
_diffrn_orient_matrix_UB_31      0.0045189
_diffrn_orient_matrix_UB_32      0.0557762
_diffrn_orient_matrix_UB_33      -0.0025185
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_unetI/netI     0.016
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13887
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    3.325
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
        (compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_density_diffrn    2.513
_exptl_crystal_density_meas      2.50(3)
_exptl_crystal_density_method    flotation
_exptl_crystal_F_000             1482
_exptl_crystal_size_max          0.2309
_exptl_crystal_size_mid          0.0935
_exptl_crystal_size_min          0.052
_refine_diff_density_max         3.423
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.302
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         3726
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0867
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+95.4386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2067
_refine_ls_wR_factor_ref         0.2069
_reflns_number_gt                3670
_reflns_number_total             3726
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4ce00264d2.cif
_cod_data_source_block           compound_1
_cod_original_cell_volume        1968.94(8)
_cod_original_formula_sum        'C3.50 H19.70 F4 Fe4 N2 O14.43 P4'
_cod_database_code               7215775