Halometallate and halide ions: nucleophiles in competition for hydrogen bond and halogen bond formation in halopyridinium salts of mixed halide‒halometallate anions
Zordan, Fiorenzo; Purver, Stephen L.; Adams, Harry; Brammer, Lee; CrystEngComm 7 (2005) 350–; doi:10.1039/b503858h

data_7203784
_publ_section_title
;
 Halometallate and halide ions: nucleophiles in competition for
 hydrogen bond and halogen bond formation in halopyridinium salts of
 mixed halide--halometallate anions
;
_journal_issue                   57
_journal_name_full               CrystEngComm
_journal_page_first              350
_journal_paper_doi               10.1039/b503858h
_journal_volume                  7
_journal_year                    2005
_chemical_formula_moiety         '3(c5 h5 br n), 2(cl4 Fe), Cl'
_chemical_formula_sum            'C15 H15 Br3 Cl9 Fe2 N3'
_chemical_formula_weight         907.78
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.716(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.583(11)
_cell_length_b                   13.960(10)
_cell_length_c                   14.695(11)
_cell_measurement_reflns_used    3908
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.29
_cell_measurement_theta_min      3.134
_cell_volume                     2990(4)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker SHELXTL'
_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      150(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  'Bruker Smart 1000 CCD'
_diffrn_measurement_method       \w-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  0.1409
_diffrn_reflns_av_sigmaI/netI    0.1412
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18984
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    5.795
_exptl_absorpt_correction_T_max  0.2585
_exptl_absorpt_correction_T_min  0.1757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.016
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.32
_refine_diff_density_max         1.817
_refine_diff_density_min         -1.678
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.909
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         7323
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0712
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1691
_refine_ls_wR_factor_ref         0.2075
_reflns_number_gt                3550
_reflns_number_total             7323
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b503858h.txt
_cod_data_source_block           ilb18m
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7203784