#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:14:33 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179833 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/29/7012968.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_7012968
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            'C19 H30 Cl2 Fe N2'
_chemical_formula_weight         413.20
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                   8.1768(19)
_cell_length_b                   13.524(2)
_cell_length_c                   37.608(6)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      4.85
_cell_volume                     4158.8(13)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Bruker 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3401
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        3.91
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.985
_exptl_absorpt_correction_T_max  0.9102
_exptl_absorpt_correction_T_min  0.7025
_exptl_absorpt_correction_type   'Lamina [0 0 1]'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'platy blocks'
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.462
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3401
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0375P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                1886
_reflns_number_total             3401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303094f.txt
_cod_data_source_block           Compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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        4158.9(14)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7012968
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.76912(8) 0.73134(4) 0.667374(18) 0.03847(18) Uani 1 1 d . . .
Cl1 Cl 0.9491(2) 0.85417(10) 0.66376(4) 0.0633(4) Uani 1 1 d . . .
Cl2 Cl 0.50878(16) 0.76981(10) 0.65630(4) 0.0540(3) Uani 1 1 d . . .
N1 N 0.8143(5) 0.6502(3) 0.71539(11) 0.0421(10) Uani 1 1 d . . .
C2 C 0.7902(7) 0.6786(4) 0.74906(15) 0.0512(14) Uani 1 1 d . . .
C3 C 0.8421(9) 0.6188(5) 0.77715(16) 0.072(2) Uani 1 1 d . . .
H3A H 0.8254 0.6395 0.8007 0.087 Uiso 1 1 calc R . .
C4 C 0.9164(10) 0.5311(6) 0.7707(2) 0.086(3) Uani 1 1 d . . .
H4A H 0.9500 0.4904 0.7896 0.104 Uiso 1 1 calc R . .
C5 C 0.9417(9) 0.5027(5) 0.73602(19) 0.074(2) Uani 1 1 d . . .
H5A H 0.9954 0.4431 0.7308 0.089 Uiso 1 1 calc R . .
C6 C 0.8870(7) 0.5631(4) 0.70921(16) 0.0542(15) Uani 1 1 d . . .
C7 C 0.9038(6) 0.5349(3) 0.67189(16) 0.0479(13) Uani 1 1 d . . .
H7A H 0.9478 0.4730 0.6657 0.057 Uiso 1 1 calc R . .
N7 N 0.8581(5) 0.5953(3) 0.64777(11) 0.0392(9) Uani 1 1 d . . .
C8 C 0.7127(8) 0.7761(4) 0.75529(15) 0.0654(16) Uani 1 1 d . . .
H8A H 0.7813 0.8278 0.7454 0.098 Uiso 1 1 calc R . .
H8B H 0.6999 0.7866 0.7807 0.098 Uiso 1 1 calc R . .
H8C H 0.6063 0.7777 0.7439 0.098 Uiso 1 1 calc R . .
C9 C 0.8768(6) 0.5657(4) 0.61033(14) 0.0421(12) Uani 1 1 d . . .
H9A H 0.9070 0.4948 0.6098 0.051 Uiso 1 1 calc R . .
C10 C 1.0184(7) 0.6245(4) 0.59413(15) 0.0519(13) Uani 1 1 d . . .
H10A H 1.0069 0.6940 0.6011 0.062 Uiso 1 1 calc R . .
H10B H 1.0097 0.6213 0.5682 0.062 Uiso 1 1 calc R . .
C11 C 1.1889(7) 0.5886(4) 0.60503(16) 0.0595(16) Uani 1 1 d . . .
H11A H 1.2707 0.6320 0.5941 0.071 Uiso 1 1 calc R . .
H11B H 1.1996 0.5951 0.6309 0.071 Uiso 1 1 calc R . .
C12 C 1.2269(7) 0.4820(4) 0.59468(13) 0.0522(13) Uani 1 1 d . . .
H12A H 1.3327 0.4635 0.6049 0.063 Uiso 1 1 calc R . .
H12B H 1.1437 0.4387 0.6052 0.063 Uiso 1 1 calc R . .
C13 C 1.2324(7) 0.4638(4) 0.55482(13) 0.0499(13) Uani 1 1 d . . .
H13A H 1.3351 0.4905 0.5454 0.060 Uiso 1 1 calc R . .
H13B H 1.1424 0.5000 0.5436 0.060 Uiso 1 1 calc R . .
C14 C 1.2196(7) 0.3542(4) 0.54432(15) 0.0535(14) Uani 1 1 d . . .
H14A H 1.2556 0.3467 0.5196 0.064 Uiso 1 1 calc R . .
H14B H 1.2942 0.3157 0.5593 0.064 Uiso 1 1 calc R . .
C15 C 1.0495(7) 0.3123(4) 0.54791(15) 0.0544(14) Uani 1 1 d . . .
H15A H 1.0074 0.3284 0.5716 0.065 Uiso 1 1 calc R . .
H15B H 1.0556 0.2401 0.5461 0.065 Uiso 1 1 calc R . .
C16 C 0.9285(7) 0.3507(4) 0.51994(13) 0.0505(13) Uani 1 1 d . . .
H16A H 0.9546 0.4200 0.5150 0.061 Uiso 1 1 calc R . .
H16B H 0.9454 0.3134 0.4979 0.061 Uiso 1 1 calc R . .
C17 C 0.7479(8) 0.3441(4) 0.52990(13) 0.0504(12) Uani 1 1 d . . .
H17A H 0.7210 0.2748 0.5348 0.060 Uiso 1 1 calc R . .
H17B H 0.6825 0.3651 0.5094 0.060 Uiso 1 1 calc R . .
C18 C 0.6980(7) 0.4064(4) 0.56215(15) 0.0491(13) Uani 1 1 d . . .
H18A H 0.7668 0.3879 0.5824 0.059 Uiso 1 1 calc R . .
H18B H 0.5844 0.3909 0.5683 0.059 Uiso 1 1 calc R . .
C19 C 0.7134(7) 0.5182(4) 0.55590(14) 0.0479(13) Uani 1 1 d . . .
H19A H 0.8139 0.5315 0.5425 0.057 Uiso 1 1 calc R . .
H19B H 0.6208 0.5407 0.5415 0.057 Uiso 1 1 calc R . .
C20 C 0.7169(7) 0.5771(4) 0.59069(14) 0.0531(14) Uani 1 1 d . . .
H20A H 0.6990 0.6473 0.5854 0.064 Uiso 1 1 calc R . .
H20B H 0.6274 0.5547 0.6060 0.064 Uiso 1 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 77.82(16) . . ?
N7 Fe Cl1 113.68(12) . . ?
N1 Fe Cl1 108.63(12) . . ?
N7 Fe Cl2 117.84(12) . . ?
N1 Fe Cl2 116.16(12) . . ?
Cl1 Fe Cl2 116.48(6) . . ?
C2 N1 C6 118.8(5) . . ?
C2 N1 Fe 128.7(4) . . ?
C6 N1 Fe 112.3(3) . . ?
N1 C2 C3 120.3(6) . . ?
N1 C2 C8 117.9(5) . . ?
C3 C2 C8 121.7(6) . . ?
C4 C3 C2 120.5(6) . . ?
C3 C4 C5 118.8(6) . . ?
C6 C5 C4 118.8(7) . . ?
N1 C6 C5 122.7(6) . . ?
N1 C6 C7 116.0(4) . . ?
C5 C6 C7 121.3(6) . . ?
N7 C7 C6 119.2(5) . . ?
C7 N7 C9 118.4(4) . . ?
C7 N7 Fe 114.3(4) . . ?
C9 N7 Fe 127.4(3) . . ?
N7 C9 C20 110.5(4) . . ?
N7 C9 C10 108.5(4) . . ?
C20 C9 C10 114.0(5) . . ?
C9 C10 C11 114.7(5) . . ?
C12 C11 C10 114.6(5) . . ?
C13 C12 C11 114.3(4) . . ?
C12 C13 C14 114.1(4) . . ?
C15 C14 C13 113.7(5) . . ?
C14 C15 C16 114.0(5) . . ?
C17 C16 C15 115.9(4) . . ?
C16 C17 C18 114.8(4) . . ?
C17 C18 C19 113.5(5) . . ?
C20 C19 C18 112.5(5) . . ?
C9 C20 C19 112.4(4) . . ?
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 2.111(4) . ?
Fe N1 2.145(4) . ?
Fe Cl1 2.2233(15) . ?
Fe Cl2 2.2307(16) . ?
N1 C2 1.338(7) . ?
N1 C6 1.341(7) . ?
C2 C3 1.397(8) . ?
C2 C8 1.481(8) . ?
C3 C4 1.354(10) . ?
C4 C5 1.375(10) . ?
C5 C6 1.372(8) . ?
C6 C7 1.461(8) . ?
C7 N7 1.277(6) . ?
N7 C9 1.472(7) . ?
C9 C20 1.509(8) . ?
C9 C10 1.531(7) . ?
C10 C11 1.532(8) . ?
C11 C12 1.526(8) . ?
C12 C13 1.520(7) . ?
C13 C14 1.537(7) . ?
C14 C15 1.508(8) . ?
C15 C16 1.535(8) . ?
C16 C17 1.526(8) . ?
C17 C18 1.532(7) . ?
C18 C19 1.536(7) . ?
C19 C20 1.532(7) . ?
