Synthesis and Structural Characterization of [bpyr]4[V4O4Cl12] and [bpyr]4[Bi4Cl16] grown in Ionic Liquid [bpyr][AlCl4] (bpyr = 1-Butylpyridinium)
Mahjoor, Parisa; Latturner, Susan E.; Crystal Growth & Design 9 (2009) 1385–; doi:10.1021/cg800625w

data_4511060
_publ_section_title
;
 Synthesis and Structural Characterization of [bpyr]4[V4O4Cl12] and
 [bpyr]4[Bi4Cl16] grown in Ionic Liquid [bpyr][AlCl4] (bpyr =
 1-Butylpyridinium)
;
_journal_issue                   3
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1385
_journal_paper_doi               10.1021/cg800625w
_journal_volume                  9
_journal_year                    2009
_chemical_formula_sum            'C36 H56 Cl12 N4 O4 V4'
_chemical_formula_weight         1238.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.4740(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.771(2)
_cell_length_b                   9.4505(6)
_cell_length_c                   17.5068(11)
_cell_measurement_reflns_used    34695
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.30
_cell_volume                     5199.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34695
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    1.354
_exptl_absorpt_correction_T_max  0.960
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via SADABS (Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.716
_refine_diff_density_min         -0.638
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.209
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.209
_refine_ls_R_factor_all          0.0887
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0895P)^2^+25.5794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1865
_reflns_number_gt                5666
_reflns_number_total             6481
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800625w_si_001.cif
_cod_data_source_block           pm1168blue
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4511060