Facile synthesis of amino-functionalised ferrocenes and vanadocenes
Bradley, Sam; McGowan, Patrick C.; Oughton, Karrie A.; Thornton-Pett, Mark; Walsh, Mark E.; Chemical Communications  (1999) 77–; doi:10.1039/a808685k

data_7115249
_publ_section_title
;
 Facile synthesis of amino-functionalised ferrocenes and vanadocenes
;
_journal_issue                   1
_journal_name_full               'Chemical Communications'
_journal_page_first              77
_journal_paper_doi               10.1039/a808685k
_journal_year                    1999
_chemical_formula_sum            'C22 H32 Fe N2'
_chemical_formula_weight         380.35
_chemical_name_systematic
; 
  ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             97-11-17
_audit_creation_method           'STADI4, X-RED'
_cell_angle_alpha                103.584(8)
_cell_angle_beta                 96.905(7)
_cell_angle_gamma                101.691(8)
_cell_formula_units_Z            2
_cell_length_a                   7.1259(5)
_cell_length_b                   10.7296(10)
_cell_length_c                   13.4298(11)
_cell_measurement_reflns_used    78
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      17.6
_cell_volume                     962.08(15)
_computing_cell_refinement       'STADI4 (STOE, 1996)'
_computing_data_collection       'STADI4 (STOE, 1996)'
_computing_data_reduction        'X-RED  (STOE, 1996)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'STOE STADI4 4-circle-diffractometer'
_diffrn_measurement_method
; Scan width (omega) = 1.65 - 1.80, scan ratio 2theta:omega = 1.00
  I(Net) and sigma(I) calculated according to Blessing (1987)
;
_diffrn_radiation_collimation    '0.8 mm'
_diffrn_radiation_detector       'NaI(Tl) scintillation counter'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  90
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0080
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3780
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.58
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.790
_exptl_absorpt_correction_T_max  0.7429
_exptl_absorpt_correction_T_min  0.6157
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
    Psi Scan Reflections used    Mu * R = 0.20  

    H   K   L   2Theta   Chi   Imin/Imax
    3  -2   0    17.8   -83.4    0.834
   -3   2   0    17.8    83.4    0.835
    4  -2  -1    23.3   -85.3    0.834
   -4   2   1    23.3    85.3    0.824
    5  -3   0    29.6   -85.5    0.825
   -5   3   0    29.6    85.5    0.834
    6  -4   0    36.0   -83.4    0.828
   -6   4   0    36.0    83.4    0.830
   -7   4   0    41.7    86.2    0.820
    7  -4   0    41.7   -86.2    0.786
   -8   3   2    47.1    84.3    0.821
    8  -3  -2    47.1   -84.3    0.832
;
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       block
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0647(24)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3773
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_obs          0.0248
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.4452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0695
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          3678
_reflns_number_total             3780
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            808685k.txt
_cod_data_source_block           PM1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+0.4452P] 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^)+(0.0380P)^2^+0.4452P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        962.08(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7115249
_audit_contact_author            'J. Richter'