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#$Date: 2025-08-04 10:03:09 +0300 (Mon, 04 Aug 2025) $
#$Revision: 301442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/65/7056581.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_7056581
loop_
_publ_author_name
'Singh, Ajai kumar'
'Singh, Mahabir Pratap'
'Saleem, Fariha'
'Pal, Ram Sahay'
_publ_section_title
;
 Palladacycles having normal and spiro chelate rings designed from bi- and
 tridentate ligands with indole core: structure, synthesis and
 applications as catalysts
;
_journal_issue                   19
_journal_name_full               'New J. Chem.'
_journal_page_first              11342
_journal_page_last               11352
_journal_paper_doi               10.1039/C7NJ02116J
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety         'C26 H22 Cl N5 Pd'
_chemical_formula_sum            'C26 H22 Cl N5 Pd'
_chemical_formula_weight         546.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc1n5d07
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-12-26 deposited with the CCDC.
2017-09-01 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.019(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.450(6)
_cell_length_b                   12.734(8)
_cell_length_c                   18.174(11)
_cell_measurement_reflns_used    2424
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.21
_cell_measurement_theta_min      2.31
_cell_volume                     2346(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1182
_diffrn_reflns_av_sigmaI/netI    0.0872
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21242
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.929
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      1.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.741
_refine_diff_density_min         -1.220
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         4126
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1273
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0519P)²+4.5405P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1527
_refine_ls_wR_factor_ref         0.1687
_reflns_number_gt                3060
_reflns_number_total             4126
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj02116j2.cif
_cod_data_source_block           Complex2
_cod_original_cell_volume        2347(2)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7056581
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.98755(6) 0.97523(5) 0.13267(3) 0.0510(3) Uani 1 1 d .
Cl1 Cl 1.1773(3) 0.8721(2) 0.18850(14) 0.0812(8) Uani 1 1 d .
N3 N 0.9314(7) 0.8918(5) 0.0351(4) 0.0538(18) Uani 1 1 d .
N2 N 0.7348(6) 1.0607(5) 0.0328(4) 0.0471(17) Uani 1 1 d .
N1 N 1.0055(7) 1.0784(6) 0.2221(4) 0.0579(19) Uani 1 1 d .
C14 C 0.5323(9) 1.1687(8) -0.0150(5) 0.063(2) Uani 1 1 d .
H14 H 0.5046 1.1329 -0.0607 0.076 Uiso 1 1 calc R
C16 C 0.8335(8) 1.0623(7) 0.0972(5) 0.049(2) Uani 1 1 d .
C18 C 0.8246(8) 0.9085(6) -0.0244(4) 0.049(2) Uani 1 1 d .
C10 C 0.6895(8) 1.1924(7) 0.1066(5) 0.053(2) Uani 1 1 d .
C15 C 0.6464(8) 1.1406(7) 0.0379(5) 0.049(2) Uani 1 1 d .
C13 C 0.4615(9) 1.2521(8) 0.0030(6) 0.074(3) Uani 1 1 d .
H13 H 0.3847 1.2737 -0.0312 0.089 Uiso 1 1 calc R
C9 C 0.8114(8) 1.1412(7) 0.1449(5) 0.052(2) Uani 1 1 d .
C22 C 0.8464(10) 0.5098(9) -0.1271(7) 0.080(3) Uani 1 1 d .
H22 H 0.8795 0.5169 -0.1700 0.096 Uiso 1 1 calc R
N5 N 0.9294(7) 0.7706(6) -0.0454(4) 0.0564(19) Uani 1 1 d .
C8 C 0.9104(9) 1.1449(8) 0.2140(5) 0.060(2) Uani 1 1 d .
H8 H 0.9067 1.1933 0.2517 0.072 Uiso 1 1 calc R
C12 C 0.5034(10) 1.3041(8) 0.0715(6) 0.076(3) Uani 1 1 d .
H12 H 0.4531 1.3597 0.0823 0.091 Uiso 1 1 calc R
C19 C 0.8239(8) 0.8314(7) -0.0752(5) 0.056(2) Uani 1 1 d .
H19 H 0.7630 0.8220 -0.1214 0.067 Uiso 1 1 calc R
C6 C 1.4381(12) 1.1878(14) 0.2657(7) 0.106(5) Uani 1 1 d .
H6 H 1.5147 1.1625 0.2545 0.128 Uiso 1 1 calc R
C2 C 1.2220(8) 1.1550(10) 0.2881(5) 0.063(3) Uani 1 1 d .
C7 C 1.3370(11) 1.1184(10) 0.2719(5) 0.088(3) Uani 1 1 d .
H7 H 1.3474 1.0468 0.2651 0.105 Uiso 1 1 calc R
C1 C 1.1123(9) 1.0830(9) 0.2930(5) 0.075(3) Uani 1 1 d .
H1A H 1.0750 1.1057 0.3342 0.090 Uiso 1 1 calc R
H1B H 1.1477 1.0129 0.3049 0.090 Uiso 1 1 calc R
C11 C 0.6181(9) 1.2764(8) 0.1249(5) 0.066(3) Uani 1 1 d .
H11 H 0.6455 1.3123 0.1705 0.080 Uiso 1 1 calc R
C5 C 1.4236(13) 1.2906(14) 0.2761(7) 0.102(4) Uani 1 1 d .
H5 H 1.4919 1.3362 0.2735 0.123 Uiso 1 1 calc R
C3 C 1.2115(10) 1.2621(10) 0.2958(5) 0.080(3) Uani 1 1 d .
H3 H 1.1344 1.2893 0.3051 0.096 Uiso 1 1 calc R
C4 C 1.3104(13) 1.3300(11) 0.2902(7) 0.103(4) Uani 1 1 d .
H4 H 1.3006 1.4019 0.2960 0.124 Uiso 1 1 calc R
N4 N 0.9944(7) 0.8072(6) 0.0222(4) 0.0572(19) Uani 1 1 d .
C26 C 0.8249(10) 0.5730(8) -0.0075(5) 0.067(3) Uani 1 1 d .
H26 H 0.8453 0.6223 0.0313 0.080 Uiso 1 1 calc R
C20 C 0.9691(10) 0.6720(8) -0.0748(6) 0.076(3) Uani 1 1 d .
H20A H 1.0574 0.6538 -0.0463 0.091 Uiso 1 1 calc R
H20B H 0.9717 0.6817 -0.1273 0.091 Uiso 1 1 calc R
C21 C 0.8775(8) 0.5836(7) -0.0697(5) 0.053(2) Uani 1 1 d .
C25 C 0.7426(12) 0.4907(9) -0.0021(7) 0.088(3) Uani 1 1 d .
H25 H 0.7065 0.4847 0.0397 0.106 Uiso 1 1 calc R
C24 C 0.7145(12) 0.4176(10) -0.0590(9) 0.103(4) Uani 1 1 d .
H24 H 0.6593 0.3614 -0.0557 0.123 Uiso 1 1 calc R
C23 C 0.7678(13) 0.4271(10) -0.1211(9) 0.108(4) Uani 1 1 d .
H23 H 0.7497 0.3764 -0.1590 0.130 Uiso 1 1 calc R
C17 C 0.7278(9) 0.9973(6) -0.0331(5) 0.056(2) Uani 1 1 d .
H17A H 0.7406 1.0424 -0.0737 0.068 Uiso 1 1 calc R
H17B H 0.6395 0.9683 -0.0488 0.068 Uiso 1 1 calc R
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'
Pd Pd -0.9988 1.0072 '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
C16 Pd1 N3 88.2(3)
C16 Pd1 N1 78.9(3)
N3 Pd1 N1 167.0(3)
C16 Pd1 Cl1 174.5(3)
N3 Pd1 Cl1 96.8(2)
N1 Pd1 Cl1 96.2(2)
N4 N3 C18 109.6(7)
N4 N3 Pd1 122.3(5)
C18 N3 Pd1 128.1(6)
C16 N2 C15 108.1(7)
C16 N2 C17 127.1(7)
C15 N2 C17 124.5(7)
C8 N1 C1 118.0(8)
C8 N1 Pd1 114.1(6)
C1 N1 Pd1 127.8(6)
C13 C14 C15 117.1(9)
N2 C16 C9 110.0(7)
N2 C16 Pd1 132.5(7)
C9 C16 Pd1 117.4(6)
C19 C18 N3 107.2(7)
C19 C18 C17 125.9(7)
N3 C18 C17 126.9(7)
C15 C10 C11 120.4(8)
C15 C10 C9 105.8(8)
C11 C10 C9 133.8(8)
C14 C15 C10 122.6(9)
C14 C15 N2 128.1(8)
C10 C15 N2 109.4(7)
C14 C13 C12 120.7(9)
C16 C9 C8 112.4(8)
C16 C9 C10 106.7(7)
C8 C9 C10 140.9(9)
C23 C22 C21 120.2(11)
N4 N5 C19 110.7(7)
N4 N5 C20 120.5(7)
C19 N5 C20 128.5(8)
N1 C8 C9 117.1(9)
C13 C12 C11 122.5(9)
C18 C19 N5 106.0(8)
C5 C6 C7 119.5(13)
C3 C2 C7 116.7(11)
C3 C2 C1 121.5(10)
C7 C2 C1 121.7(11)
C2 C7 C6 120.9(12)
C2 C1 N1 113.6(8)
C10 C11 C12 116.8(9)
C6 C5 C4 121.3(14)
C4 C3 C2 122.5(11)
C5 C4 C3 119.1(13)
N3 N4 N5 106.5(6)
C25 C26 C21 121.0(10)
N5 C20 C21 112.4(8)
C26 C21 C22 119.0(10)
C26 C21 C20 120.9(8)
C22 C21 C20 120.1(9)
C24 C25 C26 119.2(12)
C25 C24 C23 120.2(12)
C22 C23 C24 120.4(12)
N2 C17 C18 116.1(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 C16 1.932(8)
Pd1 N3 2.028(7)
Pd1 N1 2.063(7)
Pd1 Cl1 2.390(3)
N3 N4 1.313(9)
N3 C18 1.369(9)
N2 C16 1.359(9)
N2 C15 1.391(10)
N2 C17 1.432(10)
N1 C8 1.287(11)
N1 C1 1.487(10)
C14 C13 1.379(12)
C14 C15 1.386(11)
C16 C9 1.382(11)
C18 C19 1.346(11)
C18 C17 1.500(11)
C10 C15 1.388(11)
C10 C11 1.389(12)
C10 C9 1.450(11)
C13 C12 1.384(13)
C9 C8 1.422(11)
C22 C23 1.356(15)
C22 C21 1.384(12)
N5 N4 1.335(9)
N5 C19 1.348(10)
N5 C20 1.464(11)
C12 C11 1.392(12)
C6 C5 1.336(17)
C6 C7 1.403(16)
C2 C3 1.378(14)
C2 C7 1.385(13)
C2 C1 1.487(13)
C5 C4 1.365(16)
C3 C4 1.370(15)
C26 C25 1.374(14)
C26 C21 1.378(12)
C20 C21 1.495(13)
C25 C24 1.368(16)
C24 C23 1.380(16)
