Tin-Capped Trinuclear Nickel Clusters: Redox Isomerism between μ3-Stannyl and μ3-Stannylene Clusters of the Class [Ni3(dppm)3(μ3-I)(μ3-SnClx)]n+ (x= 2,n= 1;x= 3,n= 0)
Brian K. Breedlove; Philip E. Fanwick; Clifford P. Kubiak; Inorganic Chemistry 41 (2002) 4306–4308; doi:10.1021/ic020108a

data_4318386
_publ_contact_author_address
;    Department of Chemistry
      Purdue University
      W. Lafayette
      IN 47907
      USA
;
_publ_contact_author_email       fanwick@.xray.chem.purdue.edu
_publ_contact_author_fax         1(765)4940239
_publ_contact_author_name        'Phillip E. Fanwick'
_publ_contact_author_phone       1(765)4944572
_publ_section_title
;
 Tin-Capped Trinuclear Nickel Clusters: Redox Isomerism between
 \m3-Stannyl and \m3-Stannylene Clusters of the Class
 [Ni3(dppm)3(\m3-I)(\m3-SnClx)]n+ (x= 2,n= 1;x= 3,n= 0)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4306
_journal_page_last               4308
_journal_paper_doi               10.1021/ic020108a
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C87 H90 Cl3 I Ni3 O3 P6 Sn'
_chemical_formula_weight         1897.61
_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_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                69.8506(15)
_cell_angle_beta                 89.1702(15)
_cell_angle_gamma                78.010(3)
_cell_formula_units_Z            2
_cell_length_a                   14.4869(5)
_cell_length_b                   14.8724(6)
_cell_length_c                   20.4779(9)
_cell_measurement_reflns_used    23906
_cell_measurement_temperature    149
_cell_measurement_theta_max      22
_cell_measurement_theta_min      5
_cell_volume                     4043.8(3)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
     ORTEP (Johnson, 1976)
     PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF92,_Beurskins,_1992)
_diffrn_ambient_temperature      149
_diffrn_measurement_device_type  Nonius_KappaCCD
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            23906
_diffrn_reflns_theta_max         22.52
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    1.641
_exptl_absorpt_correction_T_max  0.9212
_exptl_absorpt_correction_T_min  0.5555
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.56
_exptl_crystal_description       plate
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.18
_refine_diff_density_min         -1.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     862
_refine_ls_number_reflns         10334
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.060
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0636P)^2^+21.9374P] where P=(Fo^2^+2Fc^2^)/3 '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.140
_reflns_number_gt                8573
_reflns_number_total             10334
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            ic020108a_1.cif
_cod_data_source_block           KUB011
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc ' changed to 'calc'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4043.8(4)
_cod_original_formula_sum        'C87 H90 Cl3 I1 Ni3 O3 P6 Sn1'
_cod_database_code               4318386