Spirocyclic Sulfur and Selenium Ligands as Molecular Rigid Rods in Coordination of Transition Metal Centers
Marina A. Petrukhina; Colin Henck; Bo Li; Eric Block; Jin Jin; Shao-Zhong Zhang; Rodolphe Clerac; Inorganic Chemistry 44 (2005) 77–84; doi:10.1021/ic040102g

data_4308320
_publ_section_title
;
Spirocyclic Sulfur and Selenium Ligands as Molecular Rigid Rods in
Coordination of Transition Metal Centers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              77
_journal_page_last               84
_journal_paper_doi               10.1021/ic040102g
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety
;
  [Ni (C5 O2 F6 H)2 (Se2 C5 H8)]
;
_chemical_formula_sum            'C15 H10 F12 Ni O4 Se2'
_chemical_formula_weight         698.83
_chemical_melting_point          ?
_chemical_name_systematic
;
  catena-(bis(hexafluoroacetylacetonato)-nickel(II)
  -(mu2-2,6-diselenaspiro[3,3]heptane-Se,Se'))
;
_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                 90.667(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.5479(10)
_cell_length_b                   18.739(3)
_cell_length_c                   15.885(2)
_cell_measurement_reflns_used    12220
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.52
_cell_volume                     2246.6(5)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Brucker SMART APEX CCD'
_diffrn_measurement_method       '0.3 deg wide \w exposures'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0315
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18741
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         'none (area dectector data)'
_exptl_absorpt_coefficient_mu    4.223
_exptl_absorpt_correction_T_max  0.8838
_exptl_absorpt_correction_T_min  0.2968
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.479
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5259
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0865
_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^)+(0.0366P)^2^+58.3088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2186
_refine_ls_wR_factor_ref         0.2214
_reflns_number_gt                4562
_reflns_number_total             5259
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040102g_1.cif
_cod_data_source_block           '[Ni(C5O2F6H)2(Se2C5H8)]_(10)'
_cod_depositor_comments
;
The following automatic conversions were performed:
_chemical_melting_point value 'not measured' changed to '?' - value
is undefined or not given.
Automatic conversion script
Id: cif_fix_values 1382 2010-08-28 14:56:29Z saulius 
;
_cod_original_cell_volume        2246.7(5)
_cod_database_code               4308320