Orientation and Stereodynamic Paths of Planar Monodentate Ligands in Square Planar Nickel N2S Complexes
Roxanne M. Jenkins; Michael L. Singleton; Lauren A. Leamer; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Inorganic Chemistry 49 (2010) 5503–5514; doi:10.1021/ic1002012

data_4315750
_publ_section_title
;
 Orientation and Stereodynamic Paths of Planar Monodentate Ligands in
 Square Planar Nickel N2S Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5503
_journal_page_last               5514
_journal_paper_doi               10.1021/ic1002012
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C21 H42 B2 F8 N6 Ni2 S2'
_chemical_formula_weight         733.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 100.339(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.805(5)
_cell_length_b                   14.125(7)
_cell_length_c                   20.169(10)
_cell_measurement_temperature    293(2)
_cell_volume                     3028(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.4928
_diffrn_reflns_av_sigmaI/netI    0.4766
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19669
_diffrn_reflns_theta_full        58.82
_diffrn_reflns_theta_max         58.82
_diffrn_reflns_theta_min         5.36
_exptl_absorpt_coefficient_mu    3.498
_exptl_absorpt_correction_T_max  0.9659
_exptl_absorpt_correction_T_min  0.4201
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         3867
_refine_ls_number_restraints     210
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.3079
_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 
 [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0200P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.1568
_reflns_number_gt                996
_reflns_number_total             3867
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1002012_si_007.cif
_cod_data_source_block           rx13
_cod_database_code               4315750