Crystal structure of dichlorido(4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane)iron(III) hexafluoridophosphate
Funwie, Neil L.; Cain, Amy N.; Fanning, Brian Z.; Hageman, Serena A.; Mullens, Malorie; Roberts, Travis K.; Turner, Daniel J.; Valdez, Cammi N.; Vaughan, Robert W.; Ermias, Henok G.; Silversides, Jon D.; Archibald, Stephen J.; Hubin, Timothy J.; Prior, Timothy J.; Acta Crystallographica Section E 71 (2015) 1073–1076; doi:10.1107/S2056989015015340

data_2241051
_publ_section_title
;
 Crystal structure of
 dichlorido(4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane)iron(III)
 hexafluoridophosphate
;
_journal_coeditor_code           ZL2640
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1073
_journal_page_last               1076
_journal_paper_doi               10.1107/S2056989015015340
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe Cl2 (C14 H30 N4)] P F6'
_chemical_formula_moiety         'C14 H30 Cl2 Fe N4 +, P F6 -'
_chemical_formula_sum            'C14 H30 Cl2 F6 Fe N4 P'
_chemical_formula_weight         526.14
_chemical_name_systematic
;
Dichlorido(4,11-dimethyl-1,4,8,11-tetraazabicyclo[6.6.2]hexadecane)iron(III)
hexafluoridophosphate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.002(4)
_cell_length_b                   8.5752(15)
_cell_length_c                   9.3829(16)
_cell_measurement_reflns_used    8849
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.06
_cell_measurement_theta_min      1.65
_cell_volume                     2092.1(6)
_computing_cell_refinement
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_collection
;
X-AREA (Stoe & Cie, 2002)
;
_computing_data_reduction
;
X-AREA (Stoe & Cie, 2002)
;
_computing_molecular_graphics
;
ORTEP3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2014/7 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1434
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.142
_diffrn_reflns_theta_min         1.566
_exptl_absorpt_coefficient_mu    1.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.070
_refine_diff_density_max         0.391
_refine_diff_density_min         -0.333
_refine_ls_abs_structure_details
;
 Refined as a two-component inversion twin
;
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4186
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0378P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                2249
_reflns_number_total             4186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2640sup1.cf
_cod_data_source_block           I
_cod_database_code               2241051
_shelx_estimated_absorpt_t_min   0.878
_shelx_estimated_absorpt_t_max   0.926
_shelx_hkl_checksum              77692
_shelx_res_checksum              72985
_cod_database_fobs_code 2241051