#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/28/7012856.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_7012856
loop_
_publ_author_name
'Gibson, Vernon C.'
'Spitzmesser, Stefan K.'
'White, Andrew J. P.'
'Williams, David J.'
_publ_section_title
;
 Synthesis and reactivity of 1,8-bis(imino)carbazolide complexes of
 iron, cobalt and manganese
;
_journal_issue                   13
_journal_name_full               'Dalton Transactions'
_journal_page_first              2718
_journal_paper_doi               10.1039/b301902k
_journal_year                    2003
_chemical_formula_sum            'C28 H22 Cl2 Fe N3'
_chemical_formula_weight         527.24
_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                94.896(6)
_cell_angle_beta                 101.507(7)
_cell_angle_gamma                97.380(5)
_cell_formula_units_Z            2
_cell_length_a                   9.4774(5)
_cell_length_b                   11.4602(6)
_cell_length_c                   11.7408(8)
_cell_measurement_reflns_used    26
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.82
_cell_measurement_theta_min      10.77
_cell_volume                     1231.11(13)
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3904
_diffrn_reflns_theta_max         59.99
_diffrn_reflns_theta_min         3.87
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.072
_exptl_absorpt_correction_T_max  0.3237
_exptl_absorpt_correction_T_min  0.1949
_exptl_absorpt_correction_type   Ellispoidal
_exptl_crystal_colour            'Deep red'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prisms
_exptl_crystal_F_000             542
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         3471
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.0623
_refine_ls_R_factor_obs          0.0454
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0628P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1128
_refine_ls_wR_factor_obs         0.1029
_reflns_number_observed          2962
_reflns_number_total             3649
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b301902k.txt
_cod_data_source_block           Compound_9c
_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^)+(0.0628P)^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^)+(0.0628P)^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        1231.11(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C28 H22 N3 Cl2 Fe'
_cod_database_code               7012856
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 0.31988(6) 0.63063(5) 0.27212(5) 0.0359(2) Uani 1 d . .
Cl1 Cl 0.36103(10) 0.70345(8) 0.46060(8) 0.0477(2) Uani 1 d . .
Cl2 Cl 0.10213(10) 0.58916(9) 0.15046(9) 0.0509(2) Uani 1 d . .
N1 N 0.4836(3) 0.6041(3) 0.1993(3) 0.0368(6) Uani 1 d . .
C2 C 0.5422(4) 0.4991(3) 0.1883(3) 0.0374(7) Uani 1 d . .
C3 C 0.5047(4) 0.3931(3) 0.2347(3) 0.0404(8) Uani 1 d . .
C4 C 0.5828(4) 0.2998(3) 0.2144(3) 0.0445(8) Uani 1 d . .
H4A H 0.5608(4) 0.2292(3) 0.2451(3) 0.053 Uiso 1 calc R .
C5 C 0.6914(4) 0.3084(4) 0.1503(4) 0.0460(8) Uani 1 d . .
C6 C 0.7268(4) 0.4143(4) 0.1055(3) 0.0444(8) Uani 1 d . .
H6A H 0.8005(4) 0.4221(4) 0.0637(3) 0.053 Uiso 1 calc R .
C7 C 0.6515(4) 0.5086(3) 0.1234(3) 0.0393(7) Uani 1 d . .
C8 C 0.6630(4) 0.6282(3) 0.0917(3) 0.0387(7) Uani 1 d . .
C9 C 0.7495(4) 0.6907(4) 0.0281(3) 0.0462(8) Uani 1 d . .
H9A H 0.8167(4) 0.6540(4) -0.0041(3) 0.055 Uiso 1 calc R .
C10 C 0.7363(4) 0.8068(4) 0.0124(4) 0.0515(9) Uani 1 d . .
C11 C 0.6350(5) 0.8601(4) 0.0620(4) 0.0504(9) Uani 1 d . .
H11A H 0.6261(5) 0.9385(4) 0.0515(4) 0.061 Uiso 1 calc R .
C12 C 0.5457(4) 0.7996(4) 0.1273(3) 0.0443(8) Uani 1 d . .
C13 C 0.5586(4) 0.6817(3) 0.1393(3) 0.0388(7) Uani 1 d . .
C14 C 0.3944(4) 0.3757(3) 0.3018(3) 0.0402(7) Uani 1 d . .
H14A H 0.3820(4) 0.3038(3) 0.3325(3) 0.048 Uiso 1 calc R .
N14 N 0.3105(3) 0.4519(3) 0.3231(3) 0.0390(6) Uani 1 d . .
C15 C 0.2688(2) 0.3925(3) 0.5103(2) 0.0480(9) Uani 1 d G .
H15A H 0.3690(2) 0.4048(3) 0.5391(2) 0.058 Uiso 1 calc R .
C16 C 0.1755(3) 0.3517(3) 0.5806(2) 0.0530(9) Uani 1 d G .
H16A H 0.2133(3) 0.3367(4) 0.6564(2) 0.064 Uiso 1 calc R .
C17 C 0.0258(2) 0.3334(2) 0.5376(2) 0.0502(9) Uani 1 d G .
H17A H -0.0366(3) 0.3061(4) 0.5846(3) 0.060 Uiso 1 calc R .
C18 C -0.0307(2) 0.3558(3) 0.4243(2) 0.0515(9) Uani 1 d G .
H18A H -0.1308(2) 0.3435(4) 0.3955(3) 0.062 Uiso 1 calc R .
C19 C 0.0626(2) 0.3966(2) 0.3540(2) 0.0471(9) Uani 1 d G .
H19A H 0.0248(3) 0.4116(4) 0.2782(2) 0.057 Uiso 1 calc R .
C20 C 0.2123(2) 0.4149(2) 0.3970(2) 0.0402(7) Uani 1 d G .
C21 C 0.7713(5) 0.2052(4) 0.1293(5) 0.0613(11) Uani 1 d . .
H21A H 0.7057(5) 0.1323(4) 0.1211(5) 0.092 Uiso 1 d R .
H21B H 0.8510(5) 0.2061(4) 0.1945(5) 0.092 Uiso 1 d R .
H21C H 0.8079(5) 0.2115(4) 0.0592(5) 0.092 Uiso 1 d R .
C22 C 0.8277(6) 0.8758(5) -0.0591(5) 0.0731(14) Uani 1 d . .
H22A H 0.8426(6) 0.9585(5) -0.0309(5) 0.110 Uiso 1 d R .
H22B H 0.7781(6) 0.8644(5) -0.1398(5) 0.110 Uiso 1 d R .
H22C H 0.9202(6) 0.8482(5) -0.0519(5) 0.110 Uiso 1 d R .
C23 C 0.4446(4) 0.8617(3) 0.1767(4) 0.0464(8) Uani 1 d . .
H23A H 0.4486(4) 0.9419(3) 0.1684(4) 0.056 Uiso 1 calc R .
N23 N 0.3502(4) 0.8167(3) 0.2306(3) 0.0429(7) Uani 1 d . .
C24 C 0.1187(3) 0.8813(3) 0.2499(3) 0.0658(12) Uani 1 d G .
H24A H 0.0689(3) 0.8184(3) 0.1955(3) 0.079 Uiso 1 calc R .
C25 C 0.0421(3) 0.9597(3) 0.3003(4) 0.088(2) Uani 1 d G .
H25A H -0.0591(3) 0.9492(5) 0.2796(5) 0.105 Uiso 1 calc R .
C26 C 0.1166(4) 1.0538(3) 0.3815(4) 0.093(2) Uani 1 d G .
H26A H 0.0653(6) 1.1062(4) 0.4152(5) 0.112 Uiso 1 calc R .
C27 C 0.2678(4) 1.0695(3) 0.4124(3) 0.083(2) Uani 1 d G .
H27A H 0.3176(6) 1.1325(3) 0.4668(4) 0.100 Uiso 1 calc R .
C28 C 0.3444(3) 0.9912(3) 0.3621(3) 0.0640(12) Uani 1 d G .
H28A H 0.4456(3) 1.0017(4) 0.3828(4) 0.077 Uiso 1 calc R .
C29 C 0.2699(3) 0.8971(2) 0.2808(3) 0.0501(9) Uani 1 d G .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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
N1 Fe N14 89.40(12) . . ?
N1 Fe N23 88.13(12) . . ?
N14 Fe N23 174.66(12) . . ?
N1 Fe Cl2 114.38(9) . . ?
N14 Fe Cl2 92.95(9) . . ?
N23 Fe Cl2 92.38(9) . . ?
N1 Fe Cl1 120.01(9) . . ?
N14 Fe Cl1 89.66(9) . . ?
N23 Fe Cl1 87.48(9) . . ?
Cl2 Fe Cl1 125.57(4) . . ?
C13 N1 C2 105.0(3) . . ?
C13 N1 Fe 127.8(2) . . ?
C2 N1 Fe 127.0(2) . . ?
N1 C2 C7 111.9(3) . . ?
N1 C2 C3 127.6(3) . . ?
C7 C2 C3 120.5(3) . . ?
C2 C3 C4 117.1(3) . . ?
C2 C3 C14 124.1(3) . . ?
C4 C3 C14 118.8(3) . . ?
C5 C4 C3 122.9(4) . . ?
C4 C5 C6 118.9(3) . . ?
C4 C5 C21 121.1(4) . . ?
C6 C5 C21 120.0(4) . . ?
C5 C6 C7 119.8(3) . . ?
C6 C7 C2 120.7(3) . . ?
C6 C7 C8 133.5(3) . . ?
C2 C7 C8 105.7(3) . . ?
C9 C8 C13 120.6(4) . . ?
C9 C8 C7 133.5(3) . . ?
C13 C8 C7 105.9(3) . . ?
C10 C9 C8 120.5(4) . . ?
C9 C10 C11 118.7(3) . . ?
C9 C10 C22 121.2(4) . . ?
C11 C10 C22 120.1(4) . . ?
C10 C11 C12 122.5(4) . . ?
C13 C12 C11 117.7(4) . . ?
C13 C12 C23 123.3(3) . . ?
C11 C12 C23 119.0(4) . . ?
C12 C13 N1 128.4(3) . . ?
C12 C13 C8 120.0(3) . . ?
N1 C13 C8 111.5(3) . . ?
N14 C14 C3 125.4(3) . . ?
C14 N14 C20 114.6(3) . . ?
C14 N14 Fe 126.2(2) . . ?
C20 N14 Fe 118.9(2) . . ?
C16 C15 C20 120.0 . . ?
C15 C16 C17 120.0 . . ?
C18 C17 C16 120.0 . . ?
C19 C18 C17 120.0 . . ?
C18 C19 C20 120.0 . . ?
C19 C20 C15 120.0 . . ?
C19 C20 N14 120.5(2) . . ?
C15 C20 N14 119.4(2) . . ?
N23 C23 C12 126.1(4) . . ?
C23 N23 C29 116.4(3) . . ?
C23 N23 Fe 125.8(3) . . ?
C29 N23 Fe 117.3(2) . . ?
C25 C24 C29 120.0 . . ?
C26 C25 C24 120.0 . . ?
C25 C26 C27 120.0 . . ?
C26 C27 C28 120.0 . . ?
C29 C28 C27 120.0 . . ?
C28 C29 C24 120.0 . . ?
C28 C29 N23 119.3(2) . . ?
C24 C29 N23 120.7(2) . . ?
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 N1 1.959(3) . ?
Fe N14 2.179(3) . ?
Fe N23 2.223(3) . ?
Fe Cl2 2.2318(11) . ?
Fe Cl1 2.2366(11) . ?
N1 C13 1.392(5) . ?
N1 C2 1.395(5) . ?
C2 C7 1.402(5) . ?
C2 C3 1.406(5) . ?
C3 C4 1.407(5) . ?
C3 C14 1.434(5) . ?
C4 C5 1.389(6) . ?
C5 C6 1.392(6) . ?
C5 C21 1.512(6) . ?
C6 C7 1.393(5) . ?
C7 C8 1.447(5) . ?
C8 C9 1.388(5) . ?
C8 C13 1.410(5) . ?
C9 C10 1.376(6) . ?
C10 C11 1.395(6) . ?
C10 C22 1.520(5) . ?
C11 C12 1.409(5) . ?
C12 C13 1.389(6) . ?
C12 C23 1.445(6) . ?
C14 N14 1.295(5) . ?
N14 C20 1.442(3) . ?
C15 C16 1.39 . ?
C15 C20 1.39 . ?
C16 C17 1.39 . ?
C17 C18 1.39 . ?
C18 C19 1.39 . ?
C19 C20 1.39 . ?
C23 N23 1.277(5) . ?
N23 C29 1.429(4) . ?
C24 C25 1.39 . ?
C24 C29 1.39 . ?
C25 C26 1.39 . ?
C26 C27 1.39 . ?
C27 C28 1.39 . ?
C28 C29 1.39 . ?
