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_4064983
_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         'C98.50 H84.50 Cl10.50 Fe8 Ni2 O24 P4 S8 Se4'
_chemical_formula_sum            'C98.5 H84.5 Cl10.5 Fe8 Ni2 O24 P4 S8 Se4'
_chemical_formula_weight         3284.81
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.534(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.597(4)
_cell_length_b                   18.747(3)
_cell_length_c                   27.054(4)
_cell_measurement_reflns_used    38129
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.90
_cell_measurement_theta_min      1.30
_cell_volume                     13087(3)
_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_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724 CCD'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            104334
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         1.34
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.704
_exptl_absorpt_correction_T_max  0.7373
_exptl_absorpt_correction_T_min  0.6715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6536
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         1.728
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1490
_refine_ls_number_reflns         31127
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+28.3793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1157
_refine_ls_wR_factor_ref         0.1208
_reflns_number_gt                27518
_reflns_number_total             31127
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2004767_si_001.cif
_cod_data_source_block           9a
_cod_original_formula_sum        'C98.50 H84.50 Cl10.50 Fe8 Ni2 O24 P4 S8 Se4'
_cod_database_code               4064983