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_7002273
_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 H43 N2, 2(C4 H10 O), Br6 Sb'
_chemical_formula_sum            'C41 H63 Br6 N2 O2 Sb'
_chemical_formula_weight         1217.14
_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             2005-07-25T14:55:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.818(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5696(3)
_cell_length_b                   17.2589(4)
_cell_length_c                   25.3451(6)
_cell_measurement_reflns_used    23268
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     5043.0(2)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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      -0.145387E-1
_diffrn_orient_matrix_UB_12      -0.517439E-1
_diffrn_orient_matrix_UB_13      -0.170335E-1
_diffrn_orient_matrix_UB_21      0.363304E-1
_diffrn_orient_matrix_UB_22      0.01848
_diffrn_orient_matrix_UB_23      -0.321521E-1
_diffrn_orient_matrix_UB_31      0.774115E-1
_diffrn_orient_matrix_UB_32      -0.18391E-1
_diffrn_orient_matrix_UB_33      0.156168E-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  0.0625
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            27659
_diffrn_reflns_theta_full        23.07
_diffrn_reflns_theta_max         23.07
_diffrn_reflns_theta_min         3.53
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    5.333
_exptl_absorpt_correction_T_max  0.5788
_exptl_absorpt_correction_T_min  0.4238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.048
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0222P)^2^+18.0316P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                2763
_reflns_number_total             3512
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            B905929f.txt
_cod_data_source_block           (6)-jul2005_revised
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7002273