Construction of Copper Halide-Triiron Selenide Carbonyl Complexes: Synthetic, Electrochemical, and Theoretical Studies
Minghuey Shieh; Chia-Yeh Miu; Chang-Ju Lee; Wei-Cheng Chen; Yen-Yi Chu; Hui-Lung Chen; Inorganic Chemistry 47 (2008) 11018–11031; doi:10.1021/ic8012552

data_4306451
_publ_contact_author_address
;Department of Chemistry
National Taiwan Normal University,
Taipei 116, Taiwan, Republic of China
;
_publ_contact_author_email       mshieh@ntnu.edu.tw
_publ_contact_author_name        'Minghuey Shieh'
_publ_section_title
;
Construction of Copper Halide-Triiron Selenide Carbonyl Complexes:
Synthetic, Electrochemical, and Theoretical Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11018
_journal_page_last               11031
_journal_paper_doi               10.1021/ic8012552
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C25 H40 Br1 Cu1 Fe3 N2 O9 Se1'
_chemical_formula_sum            'C25 H40 Br Cu Fe3 N2 O9 Se'
_chemical_formula_weight         902.55
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_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                 113.16
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.72660(20)
_cell_length_b                   10.05860(10)
_cell_length_c                   19.96300(29)
_cell_measurement_reflns_used    26381
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     3457.26(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'HKL Denzo and Scalepack'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0626
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34793
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  0.3698
_exptl_absorpt_correction_T_min  0.2845
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.770
_refine_diff_density_min         -2.279
_refine_diff_density_rms         0.487
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0850P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1275
_reflns_number_gt                5061
_reflns_number_total             6092
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8012552_si_002_3.cif
_cod_data_source_block           1b
_cod_original_cell_volume        3457.44(7)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               4306451