New Media for Classical Coordination Chemistry: Phase Transfer of Werner and Related Polycations into Highly Nonpolar Fluorous Solvents
Subrata K. Ghosh; Ann Sullivan Ojeda; Juan Guerrero-Leal; Nattamai Bhuvanesh; John A. Gladysz; Inorganic Chemistry 52 (2013) 9369–9378; doi:10.1021/ic400945u

data_4335731
_publ_section_title
;
 New Media for Classical Coordination Chemistry: Phase Transfer of Werner
 and Related Polycations into Highly Nonpolar Fluorous Solvents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9369
_journal_page_last               9378
_journal_paper_doi               10.1021/ic400945u
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C18 H3 Br F26'
_chemical_formula_weight         793.11
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.5335(13)
_cell_length_b                   29.5335(13)
_cell_length_c                   5.5624(3)
_cell_measurement_reflns_used    9829
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      62.60
_cell_measurement_theta_min      4.24
_cell_volume                     4851.7(4)
_computing_cell_refinement
; 
  CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) 
;
_computing_data_collection       'FRAMBO (BRUKER-NONIUS, 2003)'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    Olex2
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'BRUKER GADDS D8 Discover'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            56681
_diffrn_reflns_theta_full        59.92
_diffrn_reflns_theta_max         59.92
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.348
_exptl_absorpt_correction_T_max  0.8453
_exptl_absorpt_correction_T_min  0.2451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS; (Sheldrick, 2006)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_description       column
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         3534
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+2.7768P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0466
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                3451
_reflns_number_total             3534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400945u_si_002.cif
_cod_data_source_block           jgb
_cod_database_code               4335731