#------------------------------------------------------------------------------
#$Date: 2019-11-05 11:40:59 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223312 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/15/7701595.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_7701595
loop_
_publ_author_name
'Jing, Chuyang'
'Wang, Liang'
'Mahmood, Qaiser'
'Zhao, Mengmeng'
'Zhu, Guangqian'
'Zhang, Xianhui'
'Wang, Xiaowu'
'Wang, Qinggang'
_publ_section_title
;
 Synthesis and characterization of aminopyridine iron(ii) chloride
 catalysts for isoprene polymerization: sterically controlled monomer
 enchainment.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7862
_journal_page_last               7874
_journal_paper_doi               10.1039/c9dt00452a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C28 H32 Cl4 Fe2 N4'
_chemical_formula_weight         678.07
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-04-01 deposited with the CCDC.	2019-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.782(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1785(13)
_cell_length_b                   9.3366(8)
_cell_length_c                   22.6274(18)
_cell_measurement_reflns_used    2063
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.366
_cell_measurement_theta_min      2.582
_cell_volume                     3114.3(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0451
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7713
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.582
_exptl_absorpt_coefficient_mu    1.299
_exptl_absorpt_correction_T_max  0.8811
_exptl_absorpt_correction_T_min  0.8191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_description       block
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     189
_refine_ls_number_reflns         2739
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0339
_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)+(0.0236P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0659
_refine_ls_wR_factor_ref         0.0715
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1864
_reflns_number_total             2739
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt00452a2.cif
_cod_data_source_block           1884672
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7701595
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.819
_shelx_estimated_absorpt_t_max   0.881
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.46610(3) 0.88319(4) 0.93250(2) 0.04767(15) Uani 1 1 d . . . . .
Cl1 Cl 0.42914(5) 1.11843(8) 0.96015(3) 0.0580(2) Uani 1 1 d . . . . .
Cl2 Cl 0.57132(5) 0.80241(9) 0.88347(4) 0.0653(2) Uani 1 1 d . . . . .
N1 N 0.37998(15) 0.7239(2) 0.95464(10) 0.0460(6) Uani 1 1 d . . . . .
N2 N 0.34730(14) 0.8860(2) 0.85143(10) 0.0482(6) Uani 1 1 d . . . . .
H2 H 0.361221 0.810798 0.824839 0.058 Uiso 1 1 calc R U . . .
C1 C 0.26879(19) 0.8305(3) 0.87121(13) 0.0630(9) Uani 1 1 d . . . . .
H1A H 0.226245 0.789069 0.836546 0.076 Uiso 1 1 calc R U . . .
H1B H 0.238531 0.909206 0.886267 0.076 Uiso 1 1 calc R U . . .
C2 C 0.29486(19) 0.7186(3) 0.92046(12) 0.0474(7) Uani 1 1 d . . . . .
C3 C 0.2336(2) 0.6175(3) 0.93060(14) 0.0605(8) Uani 1 1 d . . . . .
H3 H 0.174402 0.616870 0.906940 0.073 Uiso 1 1 calc R U . . .
C4 C 0.2610(2) 0.5180(3) 0.97591(16) 0.0706(10) Uani 1 1 d . . . . .
H4 H 0.220485 0.449294 0.983227 0.085 Uiso 1 1 calc R U . . .
C5 C 0.3489(2) 0.5208(3) 1.01043(14) 0.0634(9) Uani 1 1 d . . . . .
H5 H 0.369314 0.453463 1.040884 0.076 Uiso 1 1 calc R U . . .
C6 C 0.4053(2) 0.6257(3) 0.99863(13) 0.0550(8) Uani 1 1 d . . . . .
H6 H 0.464442 0.629066 1.022394 0.066 Uiso 1 1 calc R U . . .
C7 C 0.4106(2) 1.0655(4) 0.79366(14) 0.0755(10) Uani 1 1 d . . . . .
H7A H 0.457395 1.085097 0.829518 0.113 Uiso 1 1 calc R U . . .
H7B H 0.396336 1.151635 0.770124 0.113 Uiso 1 1 calc R U . . .
H7C H 0.431274 0.993703 0.769772 0.113 Uiso 1 1 calc R U . . .
C8 C 0.3273(2) 1.0127(3) 0.81177(14) 0.0635(9) Uani 1 1 d . . . . .
H8 H 0.310030 1.088759 0.836639 0.076 Uiso 1 1 calc R U . . .
C9 C 0.2470(2) 0.9931(3) 0.75763(13) 0.0550(8) Uani 1 1 d . . . . .
C10 C 0.2639(17) 0.922(4) 0.7093(16) 0.062(4) Uani 0.576(13) 1 d . U P A 1
H10 H 0.322734 0.891842 0.710757 0.074 Uiso 0.576(13) 1 calc R U P A 1
C11 C 0.1950(9) 0.8941(19) 0.6567(8) 0.068(3) Uani 0.576(13) 1 d . U P A 1
H11 H 0.207056 0.842717 0.624272 0.081 Uiso 0.576(13) 1 calc R U P A 1
C12 C 0.1074(12) 0.9459(16) 0.6548(6) 0.076(4) Uani 0.576(13) 1 d . U P A 1
H12 H 0.060269 0.928474 0.620953 0.091 Uiso 0.576(13) 1 calc R U P A 1
C13 C 0.0919(10) 1.0209(14) 0.7022(6) 0.070(3) Uani 0.576(13) 1 d . U P A 1
H13 H 0.034851 1.058598 0.701219 0.084 Uiso 0.576(13) 1 calc R U P A 1
C14 C 0.166(2) 1.041(3) 0.7540(11) 0.061(3) Uani 0.576(13) 1 d . U P A 1
H14 H 0.155480 1.091075 0.787079 0.073 Uiso 0.576(13) 1 calc R U P A 1
C10' C 0.240(2) 0.911(5) 0.703(2) 0.062(4) Uani 0.424(13) 1 d . . P A 2
H10' H 0.288817 0.858976 0.696675 0.074 Uiso 0.424(13) 1 calc R U P A 2
C11' C 0.1584(14) 0.911(3) 0.6589(11) 0.068(3) Uani 0.424(13) 1 d . . P A 2
H11' H 0.152765 0.858910 0.623210 0.081 Uiso 0.424(13) 1 calc R U P A 2
C12' C 0.0869(16) 0.988(2) 0.6687(9) 0.076(4) Uani 0.424(13) 1 d . . P A 2
H12' H 0.033108 0.987516 0.638632 0.091 Uiso 0.424(13) 1 calc R U P A 2
C13' C 0.0896(16) 1.066(2) 0.7203(7) 0.070(3) Uani 0.424(13) 1 d . . P A 2
H13' H 0.038215 1.117095 0.723696 0.084 Uiso 0.424(13) 1 calc R U P A 2
C14' C 0.163(3) 1.072(4) 0.7653(16) 0.061(3) Uani 0.424(13) 1 d . . P A 2
H14' H 0.162894 1.122765 0.800732 0.073 Uiso 0.424(13) 1 calc R U P A 2
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_3
N1 Fe1 N2 77.32(8) .
N1 Fe1 Cl2 115.24(7) .
N2 Fe1 Cl2 97.22(6) .
N1 Fe1 Cl1 112.79(6) .
N2 Fe1 Cl1 90.58(6) .
Cl2 Fe1 Cl1 131.90(3) .
N1 Fe1 Cl1 92.87(6) 5_677
N2 Fe1 Cl1 165.72(6) 5_677
Cl2 Fe1 Cl1 96.36(3) 5_677
Cl1 Fe1 Cl1 83.61(3) 5_677
Fe1 Cl1 Fe1 96.39(3) 5_677
C2 N1 C6 118.1(2) .
C2 N1 Fe1 117.01(18) .
C6 N1 Fe1 124.87(19) .
C1 N2 C8 114.0(2) .
C1 N2 Fe1 107.45(16) .
C8 N2 Fe1 121.08(17) .
C1 N2 H2 104.2 .
C8 N2 H2 104.2 .
Fe1 N2 H2 104.2 .
N2 C1 C2 112.4(2) .
N2 C1 H1A 109.1 .
C2 C1 H1A 109.1 .
N2 C1 H1B 109.1 .
C2 C1 H1B 109.1 .
H1A C1 H1B 107.9 .
N1 C2 C3 121.6(3) .
N1 C2 C1 116.6(2) .
C3 C2 C1 121.8(3) .
C4 C3 C2 119.4(3) .
C4 C3 H3 120.3 .
C2 C3 H3 120.3 .
C3 C4 C5 119.4(3) .
C3 C4 H4 120.3 .
C5 C4 H4 120.3 .
C6 C5 C4 118.1(3) .
C6 C5 H5 121.0 .
C4 C5 H5 121.0 .
N1 C6 C5 123.5(3) .
N1 C6 H6 118.3 .
C5 C6 H6 118.3 .
C8 C7 H7A 109.5 .
C8 C7 H7B 109.5 .
H7A C7 H7B 109.5 .
C8 C7 H7C 109.5 .
H7A C7 H7C 109.5 .
H7B C7 H7C 109.5 .
N2 C8 C7 111.5(2) .
N2 C8 C9 113.8(2) .
C7 C8 C9 112.7(3) .
N2 C8 H8 106.1 .
C7 C8 H8 106.1 .
C9 C8 H8 106.1 .
C14 C9 C10 118.6(14) .
C14 C9 C8 125.4(9) .
C10 C9 C8 116.1(11) .
C10' C9 C8 129.9(15) .
C10' C9 C14' 117(2) .
C8 C9 C14' 112.6(13) .
C9 C10 C11 122(2) .
C9 C10 H10 119.1 .
C11 C10 H10 119.1 .
C12 C11 C10 117.8(18) .
C12 C11 H11 121.1 .
C10 C11 H11 121.1 .
C13 C12 C11 119.9(14) .
C13 C12 H12 120.0 .
C11 C12 H12 120.0 .
C12 C13 C14 117.8(15) .
C12 C13 H13 121.1 .
C14 C13 H13 121.1 .
C9 C14 C13 124.0(12) .
C9 C14 H14 118.0 .
C13 C14 H14 118.0 .
C11' C10' C9 119(3) .
C11' C10' H10' 120.3 .
C9 C10' H10' 120.3 .
C12' C11' C10' 119(3) .
C12' C11' H11' 120.3 .
C10' C11' H11' 120.3 .
C11' C12' C13' 124(2) .
C11' C12' H12' 118.1 .
C13' C12' H12' 118.1 .
C14' C13' C12' 122(2) .
C14' C13' H13' 119.0 .
C12' C13' H13' 119.0 .
C13' C14' C9 118.0(17) .
C13' C14' H14' 121.0 .
C9 C14' H14' 121.0 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.117(2) .
Fe1 N2 2.245(2) .
Fe1 Cl2 2.2791(9) .
Fe1 Cl1 2.3868(9) .
Fe1 Cl1 2.5668(8) 5_677
N1 C2 1.339(3) .
N1 C6 1.340(3) .
N2 C1 1.464(3) .
N2 C8 1.472(3) .
N2 H2 0.9800 .
C1 C2 1.510(4) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.382(4) .
C3 C4 1.373(4) .
C3 H3 0.9300 .
C4 C5 1.376(4) .
C4 H4 0.9300 .
C5 C6 1.369(4) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 C8 1.502(4) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C8 C9 1.520(4) .
C8 H8 0.9800 .
C9 C14 1.29(3) .
C9 C10 1.35(4) .
C9 C10' 1.44(5) .
C9 C14' 1.52(4) .
C10 C11 1.41(3) .
C10 H10 0.9300 .
C11 C12 1.406(16) .
C11 H11 0.9300 .
C12 C13 1.347(12) .
C12 H12 0.9300 .
C13 C14 1.43(3) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C10' C11' 1.38(4) .
C10' H10' 0.9300 .
C11' C12' 1.36(3) .
C11' H11' 0.9300 .
C12' C13' 1.370(18) .
C12' H12' 0.9300 .
C13' C14' 1.32(5) .
C13' H13' 0.9300 .
C14' H14' 0.9300 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C5 H5 Cl2 0.93 2.95 3.867(3) 168.2 5_667 yes
C6 H6 Cl1 0.93 2.83 3.431(3) 123.2 5_677 yes
C8 H8 Cl1 0.98 2.96 3.488(3) 115.0 . yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C8 N2 C1 C2 -169.6(2)
Fe1 N2 C1 C2 -32.5(3)
C6 N1 C2 C3 1.4(4)
Fe1 N1 C2 C3 179.1(2)
C6 N1 C2 C1 -179.8(2)
Fe1 N1 C2 C1 -2.1(3)
N2 C1 C2 N1 24.7(4)
N2 C1 C2 C3 -156.5(3)
N1 C2 C3 C4 -1.4(4)
C1 C2 C3 C4 179.9(3)
C2 C3 C4 C5 0.0(5)
C3 C4 C5 C6 1.2(5)
C2 N1 C6 C5 -0.1(4)
Fe1 N1 C6 C5 -177.6(2)
C4 C5 C6 N1 -1.2(5)
C1 N2 C8 C7 179.3(2)
Fe1 N2 C8 C7 48.7(3)
C1 N2 C8 C9 -51.9(3)
Fe1 N2 C8 C9 177.47(19)
N2 C8 C9 C14 100.6(17)
C7 C8 C9 C14 -131.2(17)
N2 C8 C9 C10 -81.1(17)
C7 C8 C9 C10 47.1(18)
N2 C8 C9 C10' -74(3)
C7 C8 C9 C10' 55(3)
N2 C8 C9 C14' 105.2(19)
C7 C8 C9 C14' -126.7(19)
C14 C9 C10 C11 -3(4)
C8 C9 C10 C11 178(2)
C9 C10 C11 C12 2(4)
C10 C11 C12 C13 0(3)
C11 C12 C13 C14 -2(2)
C10 C9 C14 C13 1(4)
C8 C9 C14 C13 179.7(15)
C12 C13 C14 C9 1(3)
C8 C9 C10' C11' -179(2)
C14' C9 C10' C11' 2(5)
C9 C10' C11' C12' 0(5)
C10' C11' C12' C13' -1(4)
C11' C12' C13' C14' -1(4)
C12' C13' C14' C9 2(4)
C10' C9 C14' C13' -3(5)
C8 C9 C14' C13' 178(2)
