Synthesis and structures of β-dialdiminatoantimony(III) halides and β-dialdiminium hexahalogenoantimoniates
Hitchcock, Peter B.; Lappert, Michael F.; Li, Gang; Coles, Martyn P.; Dalton Transactions  (2009) 7820–7826; doi:10.1039/b905929f

data_7002271
_publ_section_title
;
 Synthesis and structures of \b-dialdiminatoantimony(III) halides and
 \b-dialdiminium hexahalogenoantimoniates
;
_journal_coden_ASTM              DTARAF
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              7820
_journal_page_last               7826
_journal_paper_doi               10.1039/b905929f
_journal_year                    2009
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         '4(C33 H41 I2 N2 Sb), (C4 H10 O)'
_chemical_formula_sum            'C136 H174 I8 N8 O Sb4'
_chemical_formula_weight         3439.04
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-03-14T16:34:53-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.067(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   51.0910(6)
_cell_length_b                   13.1184(2)
_cell_length_c                   21.2525(2)
_cell_measurement_reflns_used    69475
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     14164.3(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.35096E-2
_diffrn_orient_matrix_UB_12      0.741752E-1
_diffrn_orient_matrix_UB_13      0.77689E-2
_diffrn_orient_matrix_UB_21      -0.84876E-2
_diffrn_orient_matrix_UB_22      0.16068E-1
_diffrn_orient_matrix_UB_23      -0.434356E-1
_diffrn_orient_matrix_UB_31      -0.174089E-1
_diffrn_orient_matrix_UB_32      0.71196E-2
_diffrn_orient_matrix_UB_33      0.170884E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_limit_h_max       62
_diffrn_reflns_limit_h_min       -62
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            90042
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.43
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.547
_exptl_absorpt_correction_T_max  0.6970
_exptl_absorpt_correction_T_min  0.5271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6728
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.075
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         13873
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+71.0026P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0856
_refine_ls_wR_factor_ref         0.0953
_reflns_number_gt                10640
_reflns_number_total             13873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B905929f.txt
_cod_data_source_block           (3)-mar1405_revised
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002271