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_4064980
_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_sum            'C52.5 H33.5 Cl Fe4 N0 Ni O12.25 P2 S4 Se2'
_chemical_formula_weight         1525.95
_chemical_name_systematic
; 
 ? 
;
_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                 103.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.793(3)
_cell_length_b                   17.757(4)
_cell_length_c                   23.802(5)
_cell_measurement_reflns_used    14974
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9424
_cell_measurement_theta_min      1.7613
_cell_volume                     6074(2)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'rigaku saturn CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40287
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.726
_exptl_absorpt_correction_T_max  0.5854
_exptl_absorpt_correction_T_min  0.5157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Crystalclear
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3030
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.874
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.00149(14)
_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   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         10729
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0767P)^2^+17.6146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1524
_reflns_number_gt                8874
_reflns_number_total             10729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2004767_si_001.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        6075(2)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum
'C52.50 H33.50 Cl1 Fe4 N0 Ni O12.25 P2 S4 Se2'
_cod_database_code               4064980