#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:14:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179833 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012967.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7012967
loop_
_publ_author_name
'Gibson, Vernon C.'
'O'Reilly, Rachel K.'
'Wass, Duncan F.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Iron complexes bearing iminopyridine and aminopyridine ligands as
 catalysts for atom transfer radical polymerisation
;
_journal_issue                   14
_journal_name_full               'Dalton Transactions'
_journal_page_first              2824
_journal_paper_doi               10.1039/b303094f
_journal_year                    2003
_chemical_formula_sum            'C20 H28 Cl4 Fe2 N4'
_chemical_formula_weight         577.96
_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_method           SHELXL
_cell_angle_alpha                107.005(5)
_cell_angle_beta                 108.412(7)
_cell_angle_gamma                97.019(6)
_cell_formula_units_Z            1
_cell_length_a                   7.9431(7)
_cell_length_b                   8.3374(4)
_cell_length_c                   10.5045(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.39
_cell_measurement_theta_min      4.94
_cell_volume                     613.29(9)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0457
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2286
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        3.11
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  0.8305
_exptl_absorpt_correction_T_min  0.7820
_exptl_absorpt_correction_type   Ellipsoidal
_exptl_crystal_colour            Orange/red
_exptl_crystal_density_diffrn    1.565
_exptl_crystal_description       rhombs
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.024
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1979
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.057
_refine_ls_restrained_S_obs      1.071
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_obs          0.0346
_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/[σ²(Fo²)+(0.0335P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0792
_refine_ls_wR_factor_obs         0.0706
_reflns_number_observed          1653
_reflns_number_total             2116
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b303094f.txt
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] 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^)+(0.0335P)^2^+0.0000P] 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        613.29(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7012967
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe Fe 0.43665(7) 0.30097(6) 0.84457(5) 0.02965(15) Uani 1 d . .
Cl1 Cl 0.16354(12) 0.10235(13) 0.75147(10) 0.0464(2) Uani 1 d . .
Cl2 Cl 0.45893(14) 0.39534(11) 1.10183(9) 0.0435(2) Uani 1 d . .
N1 N 0.4768(4) 0.2582(3) 0.6385(3) 0.0302(6) Uani 1 d . .
C2 C 0.3805(5) 0.2899(4) 0.5227(3) 0.0368(8) Uani 1 d . .
C3 C 0.4401(6) 0.2694(5) 0.4078(4) 0.0470(10) Uani 1 d . .
H3A H 0.3733(6) 0.2938(5) 0.3284(4) 0.056 Uiso 1 calc R .
C4 C 0.5959(6) 0.2136(5) 0.4124(4) 0.0500(10) Uani 1 d . .
H4A H 0.6350(6) 0.1995(5) 0.3360(4) 0.060 Uiso 1 calc R .
C5 C 0.6954(5) 0.1783(5) 0.5311(4) 0.0446(9) Uani 1 d . .
H5A H 0.8017(5) 0.1399(5) 0.5365(4) 0.054 Uiso 1 calc R .
C6 C 0.6304(5) 0.2024(4) 0.6422(3) 0.0334(7) Uani 1 d . .
C7 C 0.7222(5) 0.1612(4) 0.7695(4) 0.0363(8) Uani 1 d . .
H7A H 0.8255(5) 0.1173(4) 0.7762(4) 0.044 Uiso 1 calc R .
N7 N 0.6622(4) 0.1849(3) 0.8710(3) 0.0313(6) Uani 1 d D .
C8 C 0.7534(5) 0.1276(5) 0.9907(4) 0.0439(9) Uani 1 d D .
H8A H 0.7501(5) 0.0059(5) 0.9522(4) 0.053 Uiso 0.85 calc PR 1
H8B H 0.6856(5) 0.1409(5) 1.0540(4) 0.053 Uiso 0.85 calc PR 1
H8C H 0.8400(5) 0.0655(5) 0.9672(4) 0.053 Uiso 0.15 d PR 2
H8D H 0.6637(5) 0.0495(5) 1.0012(4) 0.053 Uiso 0.15 d PR 2
C9 C 0.9501(6) 0.2267(6) 1.0771(5) 0.0471(11) Uani 0.85 d PD 1
H9A H 1.0171(6) 0.2171(6) 1.0135(5) 0.057 Uiso 0.85 calc PR 1
H9B H 1.0051(6) 0.1750(6) 1.1469(5) 0.057 Uiso 0.85 calc PR 1
C10 C 0.9672(9) 0.4165(8) 1.1549(7) 0.066(2) Uani 0.85 d PD 1
H10A H 1.0938(9) 0.4734(8) 1.2078(7) 0.098 Uiso 0.85 calc PR 1
H10B H 0.9033(9) 0.4269(8) 1.2196(7) 0.098 Uiso 0.85 calc PR 1
H10C H 0.9154(9) 0.4689(8) 1.0862(7) 0.098 Uiso 0.85 calc PR 1
C9' C 0.8545(29) 0.2760(26) 1.1327(18) 0.042(6) Uiso 0.15 d PD 2
H9'A H 0.7707(29) 0.3448(26) 1.1551(18) 0.051 Uiso 0.15 calc PR 2
H9'B H 0.8988(29) 0.2298(26) 1.2084(18) 0.051 Uiso 0.15 calc PR 2
C10' C 1.0137(44) 0.3896(42) 1.1272(41) 0.059(13) Uiso 0.15 d PD 2
H10D H 1.0744(44) 0.4817(42) 1.2180(41) 0.088 Uiso 0.15 calc PR 2
H10E H 0.9699(44) 0.4372(42) 1.0535(41) 0.088 Uiso 0.15 calc PR 2
H10F H 1.0979(44) 0.3223(42) 1.1067(41) 0.088 Uiso 0.15 calc PR 2
C11 C 0.2058(5) 0.3430(5) 0.5180(4) 0.0484(10) Uani 1 d . .
H11A H 0.1084(9) 0.2420(5) 0.4825(28) 0.073 Uiso 1 calc R .
H11B H 0.1788(20) 0.4085(30) 0.4557(23) 0.073 Uiso 1 calc R .
H11C H 0.2183(13) 0.4125(30) 0.6127(6) 0.073 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Fe N1 77.16(10) . . ?
N7 Fe Cl1 112.40(8) . . ?
N1 Fe Cl1 96.21(7) . . ?
N7 Fe Cl2 109.53(8) . 2_667 ?
N1 Fe Cl2 87.28(7) . 2_667 ?
Cl1 Fe Cl2 137.65(4) . 2_667 ?
N7 Fe Cl2 97.41(8) . . ?
N1 Fe Cl2 167.36(7) . . ?
Cl1 Fe Cl2 96.41(4) . . ?
Cl2 Fe Cl2 83.79(3) 2_667 . ?
Fe Cl2 Fe 96.21(3) 2_667 . ?
C2 N1 C6 119.0(3) . . ?
C2 N1 Fe 129.6(2) . . ?
C6 N1 Fe 111.2(2) . . ?
N1 C2 C3 120.5(4) . . ?
N1 C2 C11 118.1(3) . . ?
C3 C2 C11 121.4(3) . . ?
C4 C3 C2 120.2(4) . . ?
C3 C4 C5 119.7(3) . . ?
C4 C5 C6 117.5(4) . . ?
N1 C6 C5 123.0(3) . . ?
N1 C6 C7 115.5(3) . . ?
C5 C6 C7 121.4(3) . . ?
N7 C7 C6 120.9(3) . . ?
C7 N7 C8 117.7(3) . . ?
C7 N7 Fe 114.6(2) . . ?
C8 N7 Fe 127.7(2) . . ?
N7 C8 C9 113.4(3) . . ?
N7 C8 C9' 113.4(9) . . ?
C8 C9 C10 112.6(4) . . ?
C10' C9' C8 111.5(18) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe N7 2.119(3) . ?
Fe N1 2.219(3) . ?
Fe Cl1 2.2890(10) . ?
Fe Cl2 2.4029(10) 2_667 ?
Fe Cl2 2.5246(9) . ?
Cl2 Fe 2.4029(10) 2_667 ?
N1 C2 1.336(4) . ?
N1 C6 1.352(4) . ?
C2 C3 1.403(5) . ?
C2 C11 1.498(5) . ?
C3 C4 1.367(6) . ?
C4 C5 1.384(6) . ?
C5 C6 1.392(5) . ?
C6 C7 1.467(5) . ?
C7 N7 1.274(4) . ?
N7 C8 1.482(4) . ?
C8 C9 1.516(5) . ?
C8 C9' 1.52(2) . ?
C9 C10 1.520(7) . ?
C9' C10' 1.51(2) . ?
