Crystal structure, electrochemical and spectroscopic properties of the trans-K{[FeCl(NO0)(cyclam)]·[FeCl(NO+)(cyclam)]2}(PF6)6 complex
Lopes, Luiz G. F.; Sousa, Eduardo H. S.; Miranda, José C. V.; Oliveira, Cristiane P.; Carvalho, Idalina M. M.; Batista, Alzir A.; Ellena, Javier; Castellano, Eduardo E.; Nascimento, Otaciro R.; Moreira, Ícaro S.; Journal of the Chemical Society, Dalton Transactions  (2002) 1903–; doi:10.1039/b111029b

data_7011355
_publ_section_title
;
 Crystal structure, electrochemical and spectroscopic properties of the
 trans-K{[FeCl(NO0)(cyclam)]&#x00B7;[FeCl(NO+)(cyclam)]2}(PF6)6 complex
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1903
_journal_paper_doi               10.1039/b111029b
_journal_year                    2002
_chemical_formula_sum            'C15 H36 Cl1.5 F18 Fe1.5 K0.5 N7.5 O1.5 P3'
_chemical_formula_weight         936.92
_chemical_name_systematic
;
trans-K{[FeCl(NO^0^)(cyclam)].[FeCl(NO^+^)(cyclam)]~2~}(PF~6~)~6~
;
_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'
_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                 91.052(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3560(3)
_cell_length_b                   17.7110(6)
_cell_length_c                   17.9480(6)
_cell_measurement_reflns_used    19265
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      34.972
_cell_measurement_theta_min      0.998
_cell_volume                     3291.38(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\f scans and \w scans winth \k offsets'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_sigmaI/netI    0.0388
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38116
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.62
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
SORTAV (Blessing, 1995)
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.891
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1878
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     512
_refine_ls_number_reflns         5793
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0694
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0898P)^2^+1.8125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1538
_reflns_number_gt                4181
_reflns_number_total             5793
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b111029b.txt
_cod_data_source_block           s93
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        3291.4(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum
'C15 H36 Cl1.50 F18 Fe1.50 K+0.50 N7.50 O1.50 P3'
_cod_database_code               7011355