Synthetic and Structural Characterization of Linear and Macrocyclic Ni/Fe/E (E = S, Se) Cluster Complexes
Li, Ling; Song, Li-Cheng; Wang, Miao-Miao; Li, Qian-Li; Song, Hai-Bin; Organometallics 30 (2011) 4899–; doi:10.1021/om2004767

data_4064979
_publ_section_title
;
 Synthetic and Structural Characterization of Linear and Macrocyclic
 Ni/Fe/E (E = S, Se) Cluster Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4899
_journal_paper_doi               10.1021/om2004767
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C52.50 H34.50 Cl1.50 Fe4 Ni O12 P2 S4 Se2'
_chemical_formula_sum            'C52.5 H34.5 Cl1.5 Fe4 Ni O12 P2 S4 Se2'
_chemical_formula_weight         1540.69
_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                78.180(11)
_cell_angle_beta                 72.796(9)
_cell_angle_gamma                68.781(9)
_cell_formula_units_Z            4
_cell_length_a                   14.7500(14)
_cell_length_b                   18.661(2)
_cell_length_c                   24.165(3)
_cell_measurement_reflns_used    16113
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      1.50
_cell_volume                     5887.2(12)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r2'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r2 (Rigaku, 2009)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r2'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD camera'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_sigmaI/netI    0.0816
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42404
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.18
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.835
_exptl_absorpt_correction_T_max  0.6597
_exptl_absorpt_correction_T_min  0.5743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3060
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.485
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.142
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1423
_refine_ls_number_reflns         22992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.142
_refine_ls_R_factor_all          0.0943
_refine_ls_R_factor_gt           0.0752
_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^)+(0.0430P)^2^+23.0267P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                18671
_reflns_number_total             22992
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2004767_si_001.cif
_cod_data_source_block           1
_cod_original_cell_volume        5887.2(11)
_cod_original_formula_sum        'C52.50 H34.50 Cl1.50 Fe4 Ni O12 P2 S4 Se2'
_cod_database_code               4064979