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_7002299
_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         'C38 H54 Cu N2 Sb4 1+, B F4 1-'
_chemical_formula_structural     '((C19 H27 N Sb2)2 Cu) (B F4)'
_chemical_formula_sum            'C38 H54 B Cu F4 N2 Sb4'
_chemical_formula_weight         1176.18
_chemical_name_systematic
;
bis(bis(N-(2-(dimethylstibanyl)benzyl))-methanamine-Sb,Sb')-
copper(I) tetrafluoroborate
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-01-07
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 102.588(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.517(3)
_cell_length_b                   20.044(4)
_cell_length_c                   14.2102(15)
_cell_measurement_reflns_used    50216
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     4313.5(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0959
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            53978
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.95
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.003
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.873
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         9867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0499
_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^)+(0.0219P)^2^+14.1381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0949
_reflns_number_gt                6854
_reflns_number_total             9867
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b909226a.txt
_cod_data_source_block           08mj40
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7002299