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_7030646
_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
'C33 H41 Br2 N2 Sb, 0.5(C4 H10 O), 0.5 (C4 H8 O)'
_chemical_formula_sum            'C37 H50 Br2 N2 O Sb'
_chemical_formula_weight         820.36
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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             2005-06-10T14:54:29-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.5620(2)
_cell_length_b                   26.3036(3)
_cell_length_c                   20.9135(3)
_cell_measurement_reflns_used    57774
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.022
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     7460.46(18)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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      0.447174E-1
_diffrn_orient_matrix_UB_12      -0.379631E-1
_diffrn_orient_matrix_UB_13      0.16434E-2
_diffrn_orient_matrix_UB_21      0.247538E-1
_diffrn_orient_matrix_UB_22      0.145819E-1
_diffrn_orient_matrix_UB_23      0.338826E-1
_diffrn_orient_matrix_UB_31      -0.531462E-1
_diffrn_orient_matrix_UB_32      -0.251504E-1
_diffrn_orient_matrix_UB_33      0.171642E-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  0.084
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            99742
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.52
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.911
_exptl_absorpt_correction_T_max  0.6164
_exptl_absorpt_correction_T_min  0.4187
_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    1.461
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3320
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7342
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0000P)^2^+16.4302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                5268
_reflns_number_total             7342
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7002270
_cod_data_source_file            b905929f.txt
_cod_data_source_block           (2)-jun1105_revised
_cod_original_sg_symbol_H-M      Pbcn
_cod_database_code               7030646