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_4308325
_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
;
  [(Cu (C5 O2 F6 H)2)3 (S Se C5 H8)2]
;
_chemical_formula_sum            'C40 H22 Cu3 F36 O12 S2 Se2'
_chemical_formula_weight         1791.24
_chemical_melting_point          ?
_chemical_name_systematic
;
  tris(bis(hexafluoroacetylacetonato)-copper(II))
  -bis(mu2-2-thia-6-selenaspiro[3,3]heptane-Se,S)
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.251(2)
_cell_angle_beta                 98.773(2)
_cell_angle_gamma                110.096(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2238(15)
_cell_length_b                   11.4147(15)
_cell_length_c                   12.4732(17)
_cell_measurement_reflns_used    5940
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.80
_cell_measurement_theta_min      2.34
_cell_volume                     1478.4(3)
_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 0.891
_diffrn_measured_fraction_theta_max 0.891
_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  0.0242
_diffrn_reflns_av_sigmaI/netI    0.0456
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12531
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.66
_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    2.539
_exptl_absorpt_correction_T_max  0.8037
_exptl_absorpt_correction_T_min  0.6721
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             869
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.878
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6499
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0625
_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^)+(0.0609P)^2^+3.8399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1660
_refine_ls_wR_factor_ref         0.1828
_reflns_number_gt                4809
_reflns_number_total             6499
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic040102g_6.cif
_cod_data_source_block           '[(Cu(C5O2F6H)2)3(SSeC5H8)2]_(8)'
_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_database_code               4308325