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#$Date: 2025-08-21 16:09:30 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301850 $
#$URL: svn://www.crystallography.net/cod/cif/7/04/79/7047901.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.
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data_7047901
loop_
_publ_author_name
'Figueira, Cláudia A.'
'Lopes, Patrícia S.'
'Gomes, Clara S. B.'
'Gomes, Joselaine C. S.'
'Lemos, Francisco'
'Gomes, Pedro T.'
_publ_section_title
;
 New phenyl--nickel complexes of bulky 2-iminopyrrolyl chelates:
 synthesis, characterisation and application as aluminium-free catalysts
 for the production of hyperbranched polyethylene
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT02824A
_journal_year                    2018
_chemical_formula_moiety         'C38 H34 N4 Ni'
_chemical_formula_sum            'C38 H34 N4 Ni'
_chemical_formula_weight         605.40
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n'
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-09-05 deposited with the CCDC.
2018-09-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.600(3)
_cell_length_b                   11.600(3)
_cell_length_c                   23.772(6)
_cell_measurement_reflns_used    2103
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18.64
_cell_measurement_theta_min      3.02
_cell_volume                     3198.8(14)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Mercury
_computing_publication_material  enCIFer
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1516
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            36591
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.345
_diffrn_reflns_theta_min         3.428
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.639
_exptl_absorpt_correction_T_max  0.939
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.048
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2915
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.2082
_refine_ls_R_factor_gt           0.0974
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2898
_refine_ls_wR_factor_ref         0.3422
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1191
_reflns_number_total             2915
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt02824a2.cif
_cod_data_source_block           1A
_cod_original_cell_volume        3198.8(18)
_cod_database_code               7047901
_shelx_shelxl_version_number     2018/1
_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   0.883
_shelx_estimated_absorpt_t_max   0.939
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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
Ni1 Ni 0.250000 0.750000 0.37693(5) 0.0798(7) Uani 1 2 d S T P
N1 N 0.0994(5) 0.7317(6) 0.3421(3) 0.079(2) Uani 1 1 d . . .
N2 N 0.3362(5) 0.6416(5) 0.4297(2) 0.0693(17) Uani 1 1 d . . .
C2 C 0.0173(6) 0.7924(7) 0.3719(3) 0.071(2) Uani 1 1 d . . .
C3 C -0.0925(6) 0.7719(7) 0.3482(3) 0.075(2) Uani 1 1 d . . .
H3 H -0.163557 0.803823 0.360458 0.090 Uiso 1 1 calc R U .
C4 C -0.0771(6) 0.6976(6) 0.3042(3) 0.069(2) Uani 1 1 d . . .
H4 H -0.136056 0.667632 0.280592 0.083 Uiso 1 1 calc R U .
C5 C 0.0416(7) 0.6731(7) 0.2999(3) 0.076(2) Uani 1 1 d . . .
C6 C 0.4453(6) 0.6399(7) 0.4178(3) 0.075(2) Uani 1 1 d . . .
H6 H 0.498018 0.595029 0.439151 0.090 Uiso 1 1 calc R U .
C7 C 0.0992(6) 0.5979(7) 0.2585(3) 0.1421(19) Uani 1 1 d G . .
C8 C 0.0294(5) 0.5322(7) 0.2234(3) 0.1421(19) Uani 1 1 d G . .
H8 H -0.052053 0.538355 0.225940 0.171 Uiso 1 1 calc R U .
C9 C 0.0790(6) 0.4574(7) 0.1846(3) 0.1421(19) Uani 1 1 d G . .
H9 H 0.031295 0.412501 0.160644 0.171 Uiso 1 1 calc R U .
C10 C 0.1982(6) 0.4484(7) 0.1810(3) 0.1421(19) Uani 1 1 d G . .
H10 H 0.232040 0.397274 0.154452 0.171 Uiso 1 1 calc R U .
C11 C 0.2679(5) 0.5141(8) 0.2161(3) 0.1421(19) Uani 1 1 d G U .
H11 H 0.349440 0.507900 0.213557 0.171 Uiso 1 1 calc R U .
C12 C 0.2184(6) 0.5888(7) 0.2549(3) 0.1421(19) Uani 1 1 d G U .
H12 H 0.266094 0.633756 0.278854 0.171 Uiso 1 1 calc R U .
C13 C 0.2945(6) 0.5877(6) 0.4791(4) 0.071(2) Uani 1 1 d . . .
C14 C 0.3358(7) 0.6210(7) 0.5309(4) 0.078(2) Uani 1 1 d . . .
C15 C 0.2886(8) 0.5744(8) 0.5801(4) 0.096(3) Uani 1 1 d . . .
H15 H 0.313509 0.599562 0.616167 0.115 Uiso 1 1 calc R U .
C16 C 0.2029(9) 0.4890(9) 0.5746(5) 0.106(3) Uani 1 1 d . . .
H16 H 0.171611 0.454127 0.607324 0.128 Uiso 1 1 calc R U .
C17 C 0.1646(8) 0.4561(9) 0.5234(6) 0.114(4) Uani 1 1 d . . .
H17 H 0.106976 0.398007 0.521523 0.137 Uiso 1 1 calc R U .
C18 C 0.2054(7) 0.5029(8) 0.4731(5) 0.100(3) Uani 1 1 d . . .
C19 C 0.1646(9) 0.4634(10) 0.4179(4) 0.129(4) Uani 1 1 d . . .
H19A H 0.230926 0.444868 0.394035 0.193 Uiso 1 1 calc R U .
H19B H 0.118951 0.524472 0.400155 0.193 Uiso 1 1 calc R U .
H19C H 0.116713 0.394501 0.422702 0.193 Uiso 1 1 calc R U .
C20 C 0.4257(7) 0.7146(8) 0.5366(4) 0.093(3) Uani 1 1 d . . .
H20A H 0.502723 0.679901 0.536531 0.139 Uiso 1 1 calc R U .
H20B H 0.413727 0.756184 0.572033 0.139 Uiso 1 1 calc R U .
H20C H 0.418948 0.768484 0.505030 0.139 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'
Ni Ni 0.3393 1.1124 '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'
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
N1 Ni1 N1 129.6(4) 2_565 .
N1 Ni1 N2 129.5(3) 2_565 2_565
N1 Ni1 N2 83.6(3) . 2_565
N1 Ni1 N2 83.6(3) 2_565 .
N1 Ni1 N2 129.5(3) . .
N2 Ni1 N2 104.0(3) 2_565 .
C2 N1 C5 106.7(6) . .
C2 N1 Ni1 110.2(5) . .
C5 N1 Ni1 142.9(5) . .
C6 N2 C13 120.5(7) . .
C6 N2 Ni1 110.7(5) . .
C13 N2 Ni1 128.0(5) . .
N1 C2 C6 117.9(6) . 2_565
N1 C2 C3 109.3(7) . .
C6 C2 C3 132.7(8) 2_565 .
C4 C3 C2 107.1(7) . .
C4 C3 H3 126.5 . .
C2 C3 H3 126.5 . .
C3 C4 C5 108.0(6) . .
C3 C4 H4 126.0 . .
C5 C4 H4 126.0 . .
N1 C5 C4 108.8(7) . .
N1 C5 C7 123.6(7) . .
C4 C5 C7 127.6(7) . .
N2 C6 C2 117.4(7) . 2_565
N2 C6 H6 121.3 . .
C2 C6 H6 121.3 2_565 .
C8 C7 C12 120.0 . .
C8 C7 C5 117.5(6) . .
C12 C7 C5 122.5(6) . .
C7 C8 C9 120.0 . .
C7 C8 H8 120.0 . .
C9 C8 H8 120.0 . .
C10 C9 C8 120.0 . .
C10 C9 H9 120.0 . .
C8 C9 H9 120.0 . .
C9 C10 C11 120.0 . .
C9 C10 H10 120.0 . .
C11 C10 H10 120.0 . .
C12 C11 C10 120.0 . .
C12 C11 H11 120.0 . .
C10 C11 H11 120.0 . .
C11 C12 C7 120.0 . .
C11 C12 H12 120.0 . .
C7 C12 H12 120.0 . .
C14 C13 N2 119.9(6) . .
C14 C13 C18 122.2(8) . .
N2 C13 C18 117.9(8) . .
C13 C14 C15 120.2(7) . .
C13 C14 C20 121.5(7) . .
C15 C14 C20 118.1(8) . .
C14 C15 C16 117.9(9) . .
C14 C15 H15 121.0 . .
C16 C15 H15 121.0 . .
C17 C16 C15 121.1(9) . .
C17 C16 H16 119.5 . .
C15 C16 H16 119.5 . .
C16 C17 C18 123.3(9) . .
C16 C17 H17 118.3 . .
C18 C17 H17 118.3 . .
C17 C18 C19 122.3(9) . .
C17 C18 C13 115.3(9) . .
C19 C18 C13 122.3(9) . .
C18 C19 H19A 109.5 . .
C18 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C18 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
C14 C20 H20A 109.5 . .
C14 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C14 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 1.945(5) 2_565
Ni1 N1 1.945(5) .
Ni1 N2 2.038(6) 2_565
Ni1 N2 2.038(6) .
N1 C2 1.380(9) .
N1 C5 1.385(9) .
N2 C6 1.297(8) .
N2 C13 1.416(9) .
C2 C6 1.413(10) 2_565
C2 C3 1.413(9) .
C3 C4 1.368(10) .
C3 H3 0.9500 .
C4 C5 1.409(10) .
C4 H4 0.9500 .
C5 C7 1.475(9) .
C6 H6 0.9500 .
C7 C8 1.3900 .
C7 C12 1.3900 .
C8 C9 1.3900 .
C8 H8 0.9500 .
C9 C10 1.3900 .
C9 H9 0.9500 .
C10 C11 1.3900 .
C10 H10 0.9500 .
C11 C12 1.3900 .
C11 H11 0.9500 .
C12 H12 0.9500 .
C13 C14 1.376(10) .
C13 C18 1.434(11) .
C14 C15 1.402(11) .
C14 C20 1.512(11) .
C15 C16 1.409(13) .
C15 H15 0.9500 .
C16 C17 1.350(13) .
C16 H16 0.9500 .
C17 C18 1.395(13) .
C17 H17 0.9500 .
C18 C19 1.469(13) .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 H20A 0.9800 .
C20 H20B 0.9800 .
C20 H20C 0.9800 .
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
C5 N1 C2 C6 179.9(7) . 2_565
Ni1 N1 C2 C6 3.9(9) . 2_565
C5 N1 C2 C3 -0.1(9) . .
Ni1 N1 C2 C3 -176.1(5) . .
N1 C2 C3 C4 0.6(9) . .
C6 C2 C3 C4 -179.4(8) 2_565 .
C2 C3 C4 C5 -0.9(9) . .
C2 N1 C5 C4 -0.4(8) . .
Ni1 N1 C5 C4 173.4(7) . .
C2 N1 C5 C7 179.9(7) . .
Ni1 N1 C5 C7 -6.2(13) . .
C3 C4 C5 N1 0.8(9) . .
C3 C4 C5 C7 -179.6(8) . .
C13 N2 C6 C2 -172.2(7) . 2_565
Ni1 N2 C6 C2 -1.6(9) . 2_565
N1 C5 C7 C8 171.4(6) . .
C4 C5 C7 C8 -8.2(10) . .
N1 C5 C7 C12 -6.9(10) . .
C4 C5 C7 C12 173.6(6) . .
C12 C7 C8 C9 0.0 . .
C5 C7 C8 C9 -178.3(7) . .
C7 C8 C9 C10 0.0 . .
C8 C9 C10 C11 0.0 . .
C9 C10 C11 C12 0.0 . .
C10 C11 C12 C7 0.0 . .
C8 C7 C12 C11 0.0 . .
C5 C7 C12 C11 178.2(8) . .
C6 N2 C13 C14 58.1(10) . .
Ni1 N2 C13 C14 -110.7(7) . .
C6 N2 C13 C18 -124.8(8) . .
Ni1 N2 C13 C18 66.4(9) . .
N2 C13 C14 C15 175.1(7) . .
C18 C13 C14 C15 -1.9(13) . .
N2 C13 C14 C20 0.0(12) . .
C18 C13 C14 C20 -177.0(8) . .
C13 C14 C15 C16 3.3(13) . .
C20 C14 C15 C16 178.6(8) . .
C14 C15 C16 C17 -2.3(15) . .
C15 C16 C17 C18 -0.2(17) . .
C16 C17 C18 C19 178.3(11) . .
C16 C17 C18 C13 1.7(15) . .
C14 C13 C18 C17 -0.6(12) . .
N2 C13 C18 C17 -177.6(7) . .
C14 C13 C18 C19 -177.2(9) . .
N2 C13 C18 C19 5.7(13) . .
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139173601
