#------------------------------------------------------------------------------
#$Date: 2016-09-10 02:25:26 +0300 (Sat, 10 Sep 2016) $
#$Revision: 186385 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/01/7040149.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_7040149
loop_
_publ_author_name
'Liang, Qiuming'
'Janes, Trevor'
'Gjergji, Xhoana'
'Song, Datong'
_publ_section_title
;
 Iron complexes of a bidentate picolyl-NHC ligand: synthesis, structure
 and reactivity.
;
_journal_issue                   35
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13872
_journal_page_last               13880
_journal_paper_doi               10.1039/c6dt02792j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C25 H26 Br Fe N3'
_chemical_formula_weight         504.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2016-08-04 downloaded from the CCDC.
;
_cell_angle_alpha                103.803(7)
_cell_angle_beta                 96.614(8)
_cell_angle_gamma                91.387(8)
_cell_formula_units_Z            2
_cell_length_a                   8.0411(16)
_cell_length_b                   10.612(2)
_cell_length_c                   14.202(3)
_cell_measurement_reflns_used    15205
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.996
_cell_measurement_theta_min      1.979
_cell_volume                     1167.4(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.1031
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15205
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         1.979
_exptl_absorpt_coefficient_mu    2.373
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       needle
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0571P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1011
_refine_ls_wR_factor_ref         0.1193
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2326
_reflns_number_total             3992
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02792j2.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 7040145--7040152.cif.'
_cod_database_code               7040149
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Fe1 Fe 0.35135(9) 0.44355(6) 0.72691(5) 0.0345(2) Uani 1 1 d . .
Br1 Br 0.50616(7) 0.34874(5) 0.59038(4) 0.0456(2) Uani 1 1 d . .
N1 N 0.1649(5) 0.5519(4) 0.6608(3) 0.0356(11) Uani 1 1 d . .
N2 N -0.0050(5) 0.3383(4) 0.7265(3) 0.0366(11) Uani 1 1 d . .
N3 N 0.1554(6) 0.1796(4) 0.7230(3) 0.0373(11) Uani 1 1 d . .
C1 C 0.4712(7) 0.5676(5) 0.8521(4) 0.0438(14) Uani 1 1 d . .
H1A H 0.5218 0.5180 0.8979 0.053 Uiso 1 1 calc R U
H1B H 0.5607 0.6219 0.8362 0.053 Uiso 1 1 calc R U
C2 C 0.3378(7) 0.6509(5) 0.8962(4) 0.0393(14) Uani 1 1 d . .
C3 C 0.2404(7) 0.6161(5) 0.9619(4) 0.0463(15) Uani 1 1 d . .
H3A H 0.2624 0.5384 0.9822 0.056 Uiso 1 1 calc R U
C4 C 0.1122(8) 0.6909(6) 0.9990(4) 0.0570(17) Uani 1 1 d . .
H4A H 0.0496 0.6646 1.0445 0.068 Uiso 1 1 calc R U
C5 C 0.0758(8) 0.8033(6) 0.9697(5) 0.0574(17) Uani 1 1 d . .
H5A H -0.0126 0.8543 0.9941 0.069 Uiso 1 1 calc R U
C6 C 0.1689(8) 0.8402(5) 0.9052(5) 0.0556(17) Uani 1 1 d . .
H6A H 0.1446 0.9177 0.8851 0.067 Uiso 1 1 calc R U
C7 C 0.2979(7) 0.7670(5) 0.8685(4) 0.0459(15) Uani 1 1 d . .
H7A H 0.3607 0.7954 0.8240 0.055 Uiso 1 1 calc R U
C8 C 0.1615(6) 0.3120(5) 0.7311(4) 0.0342(13) Uani 1 1 d . .
C9 C -0.0075(7) 0.1301(5) 0.7139(4) 0.0472(15) Uani 1 1 d . .
H9A H -0.0418 0.0416 0.7064 0.057 Uiso 1 1 calc R U
C10 C -0.1093(7) 0.2298(5) 0.7176(4) 0.0465(15) Uani 1 1 d . .
H10A H -0.2280 0.2261 0.7146 0.056 Uiso 1 1 calc R U
C11 C -0.0621(7) 0.4729(5) 0.7386(4) 0.0431(14) Uani 1 1 d . .
H11A H -0.0235 0.5230 0.8062 0.052 Uiso 1 1 calc R U
H11B H -0.1862 0.4693 0.7299 0.052 Uiso 1 1 calc R U
C12 C -0.0005(7) 0.5441(4) 0.6686(4) 0.0369(14) Uani 1 1 d . .
C13 C -0.1154(7) 0.6043(5) 0.6148(4) 0.0454(15) Uani 1 1 d . .
H13A H -0.2320 0.5958 0.6194 0.055 Uiso 1 1 calc R U
C14 C -0.0580(8) 0.6763(5) 0.5549(4) 0.0463(15) Uani 1 1 d . .
H14A H -0.1348 0.7187 0.5184 0.056 Uiso 1 1 calc R U
C15 C 0.1098(8) 0.6863(5) 0.5483(4) 0.0453(15) Uani 1 1 d . .
H15A H 0.1515 0.7363 0.5080 0.054 Uiso 1 1 calc R U
C16 C 0.2181(7) 0.6221(5) 0.6018(4) 0.0412(14) Uani 1 1 d . .
H16A H 0.3345 0.6279 0.5965 0.049 Uiso 1 1 calc R U
C17 C 0.3034(6) 0.1067(4) 0.7345(4) 0.0348(13) Uani 1 1 d . .
C18 C 0.3882(7) 0.1235(5) 0.8281(4) 0.0397(14) Uani 1 1 d . .
C19 C 0.5284(7) 0.0526(5) 0.8394(4) 0.0451(15) Uani 1 1 d . .
H19A H 0.5891 0.0642 0.9026 0.054 Uiso 1 1 calc R U
C20 C 0.5814(8) -0.0324(5) 0.7632(5) 0.0522(16) Uani 1 1 d . .
C21 C 0.4955(8) -0.0471(5) 0.6709(5) 0.0504(17) Uani 1 1 d . .
H21A H 0.5329 -0.1071 0.6175 0.061 Uiso 1 1 calc R U
C22 C 0.3564(8) 0.0227(5) 0.6538(4) 0.0461(15) Uani 1 1 d . .
C23 C 0.2671(9) 0.0104(5) 0.5520(4) 0.066(2) Uani 1 1 d . .
H23A H 0.1479 -0.0124 0.5507 0.100 Uiso 1 1 calc R U
H23B H 0.3164 -0.0576 0.5055 0.100 Uiso 1 1 calc R U
H23C H 0.2792 0.0934 0.5338 0.100 Uiso 1 1 calc R U
C24 C 0.3325(7) 0.2146(5) 0.9173(4) 0.0474(15) Uani 1 1 d . .
H24A H 0.2097 0.2131 0.9107 0.071 Uiso 1 1 calc R U
H24B H 0.3771 0.3032 0.9227 0.071 Uiso 1 1 calc R U
H24C H 0.3747 0.1864 0.9761 0.071 Uiso 1 1 calc R U
C25 C 0.7324(8) -0.1138(6) 0.7795(6) 0.078(2) Uani 1 1 d . .
H25A H 0.8179 -0.0605 0.8285 0.118 Uiso 1 1 calc R U
H25B H 0.7795 -0.1439 0.7178 0.118 Uiso 1 1 calc R U
H25C H 0.6963 -0.1889 0.8023 0.118 Uiso 1 1 calc R U
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C8 Fe1 C1 121.9(2)
C8 Fe1 N1 88.29(18)
C1 Fe1 N1 107.66(17)
C8 Fe1 Br1 108.34(13)
C1 Fe1 Br1 120.87(16)
N1 Fe1 Br1 102.64(11)
C16 N1 C12 118.7(5)
C16 N1 Fe1 116.8(4)
C12 N1 Fe1 124.3(3)
C8 N2 C10 113.1(4)
C8 N2 C11 122.1(4)
C10 N2 C11 124.5(4)
C9 N3 C8 111.4(4)
C9 N3 C17 124.9(4)
C8 N3 C17 123.3(5)
C2 C1 Fe1 105.7(3)
C3 C2 C7 115.9(5)
C3 C2 C1 122.9(5)
C7 C2 C1 121.1(5)
C4 C3 C2 122.4(5)
C5 C4 C3 120.1(6)
C6 C5 C4 119.0(5)
C5 C6 C7 121.4(5)
C6 C7 C2 121.2(6)
N2 C8 N3 102.1(4)
N2 C8 Fe1 124.2(4)
N3 C8 Fe1 132.9(4)
C10 C9 N3 107.8(5)
C9 C10 N2 105.6(5)
N2 C11 C12 114.2(4)
N1 C12 C13 121.1(5)
N1 C12 C11 119.8(5)
C13 C12 C11 119.1(5)
C14 C13 C12 119.2(6)
C15 C14 C13 119.7(5)
C14 C15 C16 118.6(5)
N1 C16 C15 122.7(5)
C22 C17 C18 121.9(5)
C22 C17 N3 120.2(5)
C18 C17 N3 117.8(4)
C19 C18 C17 117.9(5)
C19 C18 C24 119.3(5)
C17 C18 C24 122.8(5)
C20 C19 C18 122.0(6)
C19 C20 C21 119.1(5)
C19 C20 C25 120.4(6)
C21 C20 C25 120.5(6)
C20 C21 C22 122.1(5)
C21 C22 C17 116.9(5)
C21 C22 C23 122.0(5)
C17 C22 C23 121.1(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 C8 2.060(5)
Fe1 C1 2.061(5)
Fe1 N1 2.174(4)
Fe1 Br1 2.4511(10)
N1 C16 1.342(6)
N1 C12 1.350(6)
N2 C8 1.371(6)
N2 C10 1.380(7)
N2 C11 1.489(6)
N3 C9 1.380(7)
N3 C8 1.382(6)
N3 C17 1.450(6)
C1 C2 1.504(7)
C2 C3 1.393(8)
C2 C7 1.413(7)
C3 C4 1.391(7)
C4 C5 1.382(7)
C5 C6 1.367(8)
C6 C7 1.386(7)
C9 C10 1.348(7)
C11 C12 1.502(7)
C12 C13 1.395(7)
C13 C14 1.380(8)
C14 C15 1.367(8)
C15 C16 1.387(7)
C17 C22 1.391(7)
C17 C18 1.391(7)
C18 C19 1.385(7)
C18 C24 1.520(7)
C19 C20 1.351(7)
C20 C21 1.381(8)
C20 C25 1.535(8)
C21 C22 1.387(8)
C22 C23 1.513(8)
