Preparation and properties of cyclic and open-chain Sb/N-donor ligands
Jura, Marek; Levason, William; Reid, Gillian; Webster, Michael; Dalton Transactions  (2009) 7811–7819; doi:10.1039/b909226a

data_7002298
_publ_section_title
;
 Preparation and properties of cyclic and open-chain Sb/N-donor ligands
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7811
_journal_page_last               7819
_journal_paper_doi               10.1039/b909226a
_journal_year                    2009
_chemical_formula_moiety         'C25 H42 N2 Sb2 2+, 0.333(C H Cl3), 2(I 1-)'
_chemical_formula_sum            'C25.333 H42.333 Cl I2 N2 Sb2'
_chemical_formula_weight         907.70
_chemical_name_systematic
;
{propane-1,3-diylbis[(methylimino)methylene-2,1-phenylene]}-
bis(trimethylstibonium) iodide chloroform solvate
;
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2008-12-03
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   13.7732(10)
_cell_length_b                   13.7732(10)
_cell_length_c                   29.544(3)
_cell_measurement_reflns_used    3604
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4853.7(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0955
_diffrn_reflns_av_sigmaI/netI    0.0508
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            28258
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.676
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6283
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3789
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0344
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0071P)^2^+10.3781P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0692
_reflns_number_gt                3106
_reflns_number_total             3789
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b909226a.txt
_cod_data_source_block           08mj55
_cod_original_cell_volume        4853.6(7)
_cod_database_code               7002298