Dichloro(4,10-dimethyl-1,4,7,10-tetraazabicyclo[5.5.2]tetradecane)iron(III) hexafluorophosphate
McClain II, James M.; Maples, Danny L.; Maples, Randall D.; Matz, Dallas L.; Harris, Sebastian M.; Nelson, Andrew D. L.; Silversides, Jon D.; Archibald, Stephen J.; Hubin, Timothy J.; Acta Crystallographica Section C 62 (2006) m553–m555; doi:10.1107/S0108270106040765

data_2015661
_publ_section_title
;
 Dichloro(4,10-dimethyl-1,4,7,10-tetraazabicyclo[5.5.2]tetradecane)iron(III)
 hexafluorophosphate
;
_journal_coeditor_code           SK3055
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m553
_journal_page_last               m555
_journal_paper_doi               10.1107/S0108270106040765
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Fe Cl2 (C12 H26 N4)] (F6 P)'
_chemical_formula_moiety         'C12 H26 Cl2 Fe N4 +, F6 P -'
_chemical_formula_sum            'C12 H26 Cl2 F6 Fe N4 P'
_chemical_formula_weight         498.09
_chemical_name_systematic
;
Dichloro(4,10-dimethyl-1,4,7,10-tetraazabicyclo[5.5.2]tetradecane)iron(III)
hexafluorophosphate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 120.685(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3437(12)
_cell_length_b                   19.848(2)
_cell_length_c                   14.028(2)
_cell_measurement_reflns_used    468
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      64.15
_cell_measurement_theta_min      7.59
_cell_volume                     1997.8(5)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEPIII (Johnson, 1965; Farrugia, 1997)'
_computing_publication_material  'SHELXL97 and WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Stoe IPDS-II image plate'
_diffrn_measurement_method
'69 frames at 1\% intervals, exposure time 1.5 minutes'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            13147
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         30
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.161
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.725
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         5655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0692P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                3799
_reflns_number_total             5655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            sk3055.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2015661
_cod_database_fobs_code          2015661