Chemical Excision of Tetrahedral FeSe2 Chains from the Superconductor FeSe: Synthesis, Crystal Structure, and Magnetism of Fe3Se4(en)2
Chongin Pak; Saeed Kamali; Joyce Pham; Kathleen Lee; Joshua T. Greenfield; Kirill Kovnir; Journal of the American Chemical Society 135 (2013) 19111–19114; doi:10.1021/ja410820u

data_4121388
_publ_contact_author_address
;
Department of Chemistry
University of california at Davis
One Shields Ave
Davis CA 95616 
USA
;
_publ_contact_author_email       kkovnir@ucdavis.edu
_publ_contact_author_fax         (530)7525563
_publ_contact_author_name        'Kovnir, Kirill'
_publ_contact_author_phone       (530)7528995
_publ_section_title
;
 Chemical Excision of Tetrahedral FeSe2 Chains from the Superconductor
 FeSe: Synthesis, Crystal Structure, and Magnetism of Fe3Se4(en)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19111
_journal_page_last               19114
_journal_paper_doi               10.1021/ja410820u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C4 H16 Fe3 N4 Se4'
_chemical_formula_weight         603.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           manual
_cell_angle_alpha                90.00
_cell_angle_beta                 121.075(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.205(2)
_cell_length_b                   7.9085(9)
_cell_length_c                   11.6143(14)
_cell_measurement_temperature    90(2)
_cell_volume                     1353.5(3)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    'ATOMS V6.4.1'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from \w scans'
_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  0.0782
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8288
_diffrn_reflns_theta_full        28.99
_diffrn_reflns_theta_max         28.99
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    13.902
_exptl_absorpt_correction_T_max  0.8735
_exptl_absorpt_correction_T_min  0.4428
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.962
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.237
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1795
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0837
_reflns_number_gt                1224
_reflns_number_total             1795
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja410820u_si_002.cif
_cod_data_source_block           C4H16Fe3N4Se4
_cod_original_cell_volume        1353.6(3)
_cod_database_code               4121388