Tetrahedral and Square Planar Ni[(SPR2)2N]2 complexes, R = Ph & iPr Revisited: Experimental and Theoretical Analysis of Interconversion Pathways, Structural Preferences, and Spin Delocalization
Dimitrios Maganas; Alexios Grigoropoulos; Sarah S. Staniland; Spyros D. Chatziefthimiou; Andrew Harrison; Neil Robertson; Panayotis Kyritsis; Frank Neese; Inorganic Chemistry 49 (2010) 5079–5093; doi:10.1021/ic100163g

data_4315597
_publ_contact_author_address
;
Department of Chemistry
Inorganic Chemistry Laboratory
University of Athens
GR-15771 Athens
Greece
;
_publ_contact_author_email       Kyritsis@chem.uoa.gr
_publ_contact_author_fax         '+30 210-7274782'
_publ_contact_author_name        'Panayotis Kyritsis'
_publ_contact_author_phone       +30-210-7274268
_publ_section_title
;
 Tetrahedral and Square Planar Ni[(SPR2)2N]2 complexes, R = Ph & iPr
 Revisited: Experimental and Theoretical Analysis of Interconversion
 Pathways, Structural Preferences, and Spin Delocalization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5079
_journal_page_last               5093
_journal_paper_doi               10.1021/ic100163g
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C36 H48 N2 Ni1 P4 S4'
_chemical_formula_sum            'C36 H48 N2 Ni P4 S4'
_chemical_formula_weight         819.66
_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
_audit_creation_date             04-08-13
_audit_creation_method           CRYSTALS_ver_12.39
_cell_angle_alpha                87.8670(10)
_cell_angle_beta                 88.2800(10)
_cell_angle_gamma                89.7280(10)
_cell_formula_units_Z            3
_cell_length_a                   9.1329(2)
_cell_length_b                   17.0596(4)
_cell_length_c                   19.1631(4)
_cell_measurement_reflns_used    7821
_cell_measurement_temperature    150
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2
_cell_volume                     2982.25(11)
_computing_cell_refinement       'SAINT (Siemens ,1995)'
_computing_data_collection       'SMART (Siemens, 1993)'
_computing_data_reduction        'SAINT (Siemens ,1995)'
_computing_molecular_graphics    'CAMERON (Watkin et al 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al 2003)'
_computing_structure_solution    'SIR92 (Altomare et al, 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25269
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         28.780
_diffrn_reflns_theta_min         1.064
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.44
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_description       plate
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.77
_refine_diff_density_min         -0.76
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0161
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         13081
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000440
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 p=P(6)*max(Fo^2^,0) + (1-P(6))Fc^2^ 
 Method = SHELXL 97 (Sheldrick, 1997) 
 W = 1. / [Sigma^2^(F*)+(P(1)p)^2^+P(2)p+P(4)+P(5)Sin(theta) ] 
 P(i) are: 
 0.228E-01 4.99 0.00 0.00 0.00 0.333 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1365
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1365
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              22
_reflns_limit_k_min              -22
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                10412
_reflns_number_total             13089
_reflns_threshold_expression     I>2.00u(I)
_oxford_diffrn_Wilson_B_factor   1.46
_oxford_diffrn_Wilson_scale      7.35
_oxford_refine_ls_scale          0.3116(2)
_oxford_structure_analysis_title 'sspk1a in P-1'
_cod_data_source_file            ic100163g_si_003_2.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C36 H48 N2 Ni1 P4 S4'
_cod_database_code               4315597