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_4306456
_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         'C66 H40 Br2 Cu4 Fe6 O18 P2 Se2'
_chemical_formula_sum            'C66 H40 Br2 Cu4 Fe6 O18 P2 Se2'
_chemical_formula_weight         2089.92
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.4740(10)
_cell_angle_beta                 90.8120(10)
_cell_angle_gamma                105.1420(10)
_cell_formula_units_Z            1
_cell_length_a                   11.45390(20)
_cell_length_b                   12.03890(20)
_cell_length_c                   14.28130(29)
_cell_measurement_reflns_used    30900
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.037
_cell_volume                     1814.57(6)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17531
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    4.523
_exptl_absorpt_correction_T_max  0.4796
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.913
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       0.0096(5)
_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   1.092
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0345
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0517P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0822
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                4984
_reflns_number_total             6383
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8012552_si_002_8.cif
_cod_data_source_block           3b
_cod_database_code               4306456