Synthesis of a ferrocene bridged cyclam: a new redox-active macrocycle and the structure of a nickel(II) complex with strongly coupled metal centers
Plenio, Herbert; Aberle, Clemens; Chemical Communications  (1998) 2697–; doi:10.1039/a807240j

data_7110364
_publ_section_title
;
 Synthesis of a ferrocene bridged cyclam: a new redox-active macrocycle
 and the structure of a nickel(II) complex with strongly coupled metal
 centers
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2697
_journal_paper_doi               10.1039/a807240j
_journal_year                    1998
_chemical_formula_sum            'C13.5 H20 F3 Fe0.5 N2 Ni0.5 O3.5 S'
_chemical_formula_weight         412.65
_chemical_name_common            'ferrocene cyclam x Ni(II)triflate complex'
_chemical_name_systematic
;
 1,8-(1,1'-ferrocenedimethyldiyl),4,11-tetraaza-cyclotetradecane-
  Nickel(II)triflate complex'
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                   10.5735(15)
_cell_length_b                   10.5735(15)
_cell_length_c                   30.251(6)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_volume                     3382.0(10)
_computing_cell_refinement       'turbo-mol, enraf-nonius'
_computing_data_collection       'turbo-mol, enraf-nonius'
_computing_data_reduction        'cadfor, cadsex, E. Keller, Freiburg 1993'
_computing_molecular_graphics    'Schakal, E. Keller, Freiburg 1995'
_computing_publication_material  'CIFTAB, G.M. Sheldirck'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'enraf-nonius cad4f'
_diffrn_measurement_method       omega-2theta
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0787
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            3524
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         2.69
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 'every 100 refl.'
_diffrn_standards_interval_time  'every 60 min'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.192
_exptl_absorpt_correction_type   'empirical, psi-scans'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1704
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_coef       no
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         3137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+2.0909P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1101
_refine_ls_wR_factor_ref         0.1323
_reflns_number_gt                2152
_reflns_number_total             3137
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            807240jsup1.cif
_cod_data_source_block           ca4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+2.0909P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+2.0909P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4(3)2(1)2
_cod_original_formula_sum        'C13.50 H20 F3 Fe0.50 N2 Ni0.50 O3.50 S'
_cod_database_code               7110364