Synthesis and characterisation of transition metal halide complexes of the xylyl-distibine, 1,2-bis(dimethylstibanylmethyl)benzene.
Levason, William; Matthews, Melissa L.; Reid, Gillian; Webster, Michael; Dalton transactions (Cambridge, England : 2003)  (2004) 554–561; doi:10.1039/b400214h

data_7014029
_publ_section_title
;
 Synthesis and characterisation of transition metal halide complexes of
 the xylyl-distibine, 1,2-bis(dimethylstibanylmethyl)benzene.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              554
_journal_page_last               561
_journal_paper_doi               10.1039/b400214h
_journal_year                    2004
_chemical_formula_moiety         'C24 H40 I Ni Sb4 1+, Cl O4 1-'
_chemical_formula_sum            'C24 H40 Cl I Ni O4 Sb4'
_chemical_formula_weight         1100.62
_chemical_name_systematic
;
Iodobis(1,2-bis(dimethylstibanylmethyl)benzene)nickel(II) perchlorate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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 + hand edit'
_cell_angle_alpha                95.814(10)
_cell_angle_beta                 95.740(10)
_cell_angle_gamma                107.789(8)
_cell_formula_units_Z            4
_cell_length_a                   9.4616(15)
_cell_length_b                   13.608(3)
_cell_length_c                   27.146(4)
_cell_measurement_reflns_used    47934
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     3279.1(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'area detector, Nonius Kappa ccd'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1004
_diffrn_reflns_av_sigmaI/netI    0.1030
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            38793
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    4.866
_exptl_absorpt_correction_T_max  0.88270
_exptl_absorpt_correction_T_min  0.78889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SORTAV, R H Blessing, J. Appl. Cryst., 1997, 30, 421-426.'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    2.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.759
_refine_diff_density_min         -1.889
_refine_diff_density_rms         0.268
_refine_ls_extinction_coef       0.00079(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         11251
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0586
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+3.4579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1595
_reflns_number_gt                7012
_reflns_number_total             11251
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b400214h.txt
_cod_data_source_block           niisb4
_cod_original_cell_volume        3279.2(9)
_cod_database_code               7014029