#------------------------------------------------------------------------------
#$Date: 2016-09-10 02:25:26 +0300 (Sat, 10 Sep 2016) $
#$Revision: 186385 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/01/7040151.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_7040151
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            'C21 H19 Fe N3 O3'
_chemical_formula_weight         417.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 118.981(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.764(2)
_cell_length_b                   8.8282(10)
_cell_length_c                   16.118(2)
_cell_measurement_reflns_used    24729
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.593
_cell_measurement_theta_min      1.483
_cell_volume                     1962.2(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24729
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.593
_diffrn_reflns_theta_min         1.483
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0378
_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)+(0.0639P)²+0.0928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3381
_reflns_number_total             4536
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt02792j2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7040145--7040152.cif.'
_cod_original_cell_volume        1962.3(5)
_cod_database_code               7040151
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.82280(2) 0.86634(3) 0.53381(2) 0.02225(12) Uani 1 1 d . .
O1 O 0.90992(16) 1.15215(18) 0.62389(13) 0.0518(6) Uani 1 1 d . .
O2 O 0.73984(16) 1.0624(2) 0.36683(12) 0.0533(6) Uani 1 1 d . .
O3 O 0.63501(15) 0.8410(2) 0.52492(15) 0.0538(6) Uani 1 1 d . .
N1 N 0.86353(14) 0.70256(19) 0.46768(11) 0.0253(4) Uani 1 1 d . .
N2 N 0.87360(13) 0.58010(19) 0.63624(12) 0.0232(4) Uani 1 1 d . .
N3 N 0.94132(13) 0.75423(19) 0.73997(12) 0.0233(4) Uani 1 1 d . .
C1 C 0.88414(18) 1.0309(3) 0.59312(15) 0.0306(5) Uani 1 1 d . .
C2 C 0.77212(19) 0.9812(2) 0.43129(16) 0.0332(6) Uani 1 1 d . .
C3 C 0.70920(19) 0.8396(3) 0.52656(17) 0.0333(6) Uani 1 1 d . .
C4 C 0.88379(15) 0.7339(2) 0.64489(14) 0.0210(4) Uani 1 1 d . .
C5 C 0.96537(18) 0.6156(2) 0.78790(15) 0.0279(5) Uani 1 1 d . .
H5A H 1.0045 0.6011 0.8543 0.033 Uiso 1 1 calc R U
C6 C 0.92293(17) 0.5074(2) 0.72262(15) 0.0263(5) Uani 1 1 d . .
H6A H 0.9261 0.4013 0.7335 0.032 Uiso 1 1 calc R U
C7 C 0.81660(18) 0.5082(2) 0.54427(14) 0.0275(5) Uani 1 1 d . .
H7A H 0.7478 0.5388 0.5173 0.033 Uiso 1 1 calc R U
H7B H 0.8202 0.3968 0.5523 0.033 Uiso 1 1 calc R U
C8 C 0.85282(16) 0.5519(2) 0.47744(14) 0.0262(5) Uani 1 1 d . .
C9 C 0.87207(17) 0.4432(2) 0.42672(15) 0.0312(6) Uani 1 1 d . .
H9A H 0.8651 0.3387 0.4361 0.037 Uiso 1 1 calc R U
C10 C 0.90131(18) 0.4878(3) 0.36275(16) 0.0354(6) Uani 1 1 d . .
H10A H 0.9130 0.4149 0.3260 0.042 Uiso 1 1 calc R U
C11 C 0.91339(19) 0.6398(3) 0.35290(16) 0.0337(6) Uani 1 1 d . .
H11A H 0.9338 0.6736 0.3094 0.040 Uiso 1 1 calc R U
C12 C 0.89552(18) 0.7424(3) 0.40694(15) 0.0304(5) Uani 1 1 d . .
H12A H 0.9063 0.8468 0.4011 0.036 Uiso 1 1 calc R U
C13 C 0.97327(17) 0.8969(2) 0.78890(14) 0.0243(5) Uani 1 1 d . .
C14 C 0.9165(2) 0.9647(3) 0.82223(16) 0.0344(6) Uani 1 1 d . .
C15 C 0.9522(2) 1.0977(3) 0.87511(18) 0.0415(7) Uani 1 1 d . .
H15A H 0.9153 1.1459 0.8998 0.050 Uiso 1 1 calc R U
C16 C 1.0394(2) 1.1610(3) 0.89254(16) 0.0366(6) Uani 1 1 d . .
C17 C 1.09196(18) 1.0923(2) 0.85470(15) 0.0313(6) Uani 1 1 d . .
H17A H 1.1505 1.1377 0.8640 0.038 Uiso 1 1 calc R U
C18 C 1.06079(17) 0.9577(2) 0.80325(14) 0.0270(5) Uani 1 1 d . .
C19 C 1.11935(19) 0.8837(3) 0.76363(18) 0.0359(6) Uani 1 1 d . .
H19A H 1.0779 0.8652 0.6956 0.054 Uiso 1 1 calc R U
H19B H 1.1453 0.7872 0.7962 0.054 Uiso 1 1 calc R U
H19C H 1.1730 0.9505 0.7732 0.054 Uiso 1 1 calc R U
C20 C 0.8193(2) 0.9010(4) 0.8007(2) 0.0544(8) Uani 1 1 d . .
H20A H 0.8257 0.7922 0.8145 0.082 Uiso 1 1 calc R U
H20B H 0.7728 0.9172 0.7335 0.082 Uiso 1 1 calc R U
H20C H 0.7963 0.9521 0.8400 0.082 Uiso 1 1 calc R U
C21 C 1.0778(2) 1.3029(3) 0.95189(19) 0.0547(9) Uani 1 1 d . .
H21A H 1.0272 1.3472 0.9630 0.082 Uiso 1 1 calc R U
H21B H 1.0969 1.3762 0.9183 0.082 Uiso 1 1 calc R U
H21C H 1.1342 1.2773 1.0128 0.082 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'
O O 0.0106 0.0060 '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
C1 Fe1 C3 115.11(12)
C1 Fe1 C2 85.07(10)
C3 Fe1 C2 91.75(12)
C1 Fe1 C4 95.72(9)
C3 Fe1 C4 90.79(10)
C2 Fe1 C4 176.72(11)
C1 Fe1 N1 129.24(10)
C3 Fe1 N1 115.62(10)
C2 Fe1 N1 91.82(9)
C4 Fe1 N1 85.21(8)
C12 N1 C8 116.79(19)
C12 N1 Fe1 120.62(14)
C8 N1 Fe1 122.41(15)
C4 N2 C6 112.22(16)
C4 N2 C7 121.43(16)
C6 N2 C7 126.36(17)
C4 N3 C5 111.16(17)
C4 N3 C13 126.59(17)
C5 N3 C13 122.23(17)
O1 C1 Fe1 168.5(2)
O2 C2 Fe1 176.8(2)
O3 C3 Fe1 171.4(2)
N3 C4 N2 103.11(16)
N3 C4 Fe1 135.63(15)
N2 C4 Fe1 121.26(14)
C6 C5 N3 107.01(18)
C5 C6 N2 106.51(17)
N2 C7 C8 111.04(18)
N1 C8 C9 122.3(2)
N1 C8 C7 116.61(19)
C9 C8 C7 121.1(2)
C10 C9 C8 119.5(2)
C9 C10 C11 118.7(2)
C10 C11 C12 119.1(2)
N1 C12 C11 123.4(2)
C14 C13 C18 123.0(2)
C14 C13 N3 118.1(2)
C18 C13 N3 118.9(2)
C13 C14 C15 117.0(2)
C13 C14 C20 121.7(2)
C15 C14 C20 121.2(3)
C16 C15 C14 122.1(3)
C15 C16 C17 118.8(2)
C15 C16 C21 121.2(3)
C17 C16 C21 120.0(3)
C16 C17 C18 121.4(2)
C13 C18 C17 117.5(2)
C13 C18 C19 121.73(19)
C17 C18 C19 120.7(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 C1 1.751(2)
Fe1 C3 1.753(3)
Fe1 C2 1.766(2)
Fe1 C4 1.957(2)
Fe1 N1 2.0742(18)
O1 C1 1.167(3)
O2 C2 1.157(3)
O3 C3 1.157(3)
N1 C12 1.347(3)
N1 C8 1.360(3)
N2 C4 1.367(3)
N2 C6 1.381(3)
N2 C7 1.455(3)
N3 C4 1.362(2)
N3 C5 1.398(3)
N3 C13 1.441(3)
C5 C6 1.336(3)
C7 C8 1.494(3)
C8 C9 1.386(3)
C9 C10 1.375(4)
C10 C11 1.376(3)
C11 C12 1.377(3)
C13 C14 1.384(3)
C13 C18 1.391(3)
C14 C15 1.398(3)
C14 C20 1.506(4)
C15 C16 1.380(4)
C16 C17 1.385(4)
C16 C21 1.513(3)
C17 C18 1.395(3)
C18 C19 1.502(4)
