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#$Date: 2024-03-04 22:34:45 +0200 (Mon, 04 Mar 2024) $
#$Revision: 290231 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/29/7062979.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_7062979
loop_
_publ_author_name
'Geng, Yanxue'
'Sun, Weijun'
'Zhang, Weixu'
'Li, Mengyao'
'Wang, Guo'
'Wang, Jianchun'
_publ_section_title
;
 A new class of unique quinoidal-like imidazoliumyl tetrazinides:
 synthesis, structure, and mechanism
;
_journal_issue                   8
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              3467
_journal_page_last               3471
_journal_paper_doi               10.1039/D3NJ04766K
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'Cl4 Pd, 2(C5 H9 N2)'
_chemical_formula_sum            'C10 H18 Cl4 N4 Pd'
_chemical_formula_weight         442.48
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-09-18 deposited with the CCDC.	2024-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.52(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6646(17)
_cell_length_b                   8.0989(16)
_cell_length_c                   12.187(2)
_cell_measurement_reflns_used    2961
_cell_measurement_temperature    163(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      1.7186
_cell_volume                     831.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      163.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5866
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.618
_exptl_absorpt_coefficient_mu    1.750
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.128
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1891
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0390
_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)+(0.0518P)²+1.2573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1817
_reflns_number_total             1891
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj04766k2.cif
_cod_data_source_block           bww19367
_cod_depositor_comments
'Adding full bibliography for 7062975--7062979.cif.'
_cod_database_code               7062979
_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_max   0.844
_shelx_estimated_absorpt_t_min   0.804
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 N1(H1)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.000000 0.000000 0.500000 0.03073(15) Uani 1 2 d S T P . .
Cl1 Cl -0.00968(10) 0.28086(11) 0.46900(9) 0.0418(2) Uani 1 1 d . . . . .
Cl2 Cl 0.22948(13) -0.01060(10) 0.43478(10) 0.0445(3) Uani 1 1 d . . . . .
N2 N 0.4917(4) 0.4867(4) 0.6603(3) 0.0402(8) Uani 1 1 d . . . . .
N1 N 0.6781(3) 0.6346(4) 0.6272(2) 0.0393(7) Uani 1 1 d . . . . .
H1 H 0.734515 0.719617 0.620129 0.047 Uiso 1 1 d R . . . .
C1 C 0.5427(4) 0.6375(5) 0.6614(3) 0.0371(8) Uani 1 1 d . . . . .
C2 C 0.5960(6) 0.3832(5) 0.6264(3) 0.0518(11) Uani 1 1 d . . . . .
H2 H 0.586530 0.266666 0.619078 0.062 Uiso 1 1 calc R . . . .
C3 C 0.7129(5) 0.4748(6) 0.6054(3) 0.0484(10) Uani 1 1 d . . . . .
H3 H 0.802624 0.437074 0.580336 0.058 Uiso 1 1 calc R . . . .
C4 C 0.4658(5) 0.7902(5) 0.6929(3) 0.0491(9) Uani 1 1 d . . . . .
H4A H 0.358886 0.801018 0.644253 0.074 Uiso 1 1 calc GR . . . .
H4B H 0.529302 0.886869 0.683145 0.074 Uiso 1 1 calc GR . . . .
H4C H 0.458936 0.782635 0.771842 0.074 Uiso 1 1 calc GR . . . .
C5 C 0.3434(5) 0.4361(7) 0.6910(4) 0.0540(10) Uani 1 1 d . . . . .
H5A H 0.368899 0.383012 0.765306 0.081 Uiso 1 1 calc GR . . . .
H5B H 0.285584 0.358132 0.634608 0.081 Uiso 1 1 calc GR . . . .
H5C H 0.277195 0.533567 0.693360 0.081 Uiso 1 1 calc GR . . . .
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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 Cl1 180.0 . 3_556 ?
Cl1 Pd1 Cl2 91.06(3) 3_556 . ?
Cl1 Pd1 Cl2 88.94(3) . . ?
Cl1 Pd1 Cl2 88.94(3) 3_556 3_556 ?
Cl1 Pd1 Cl2 91.06(3) . 3_556 ?
Cl2 Pd1 Cl2 180.0 3_556 . ?
C1 N2 C2 109.4(3) . . ?
C1 N2 C5 124.9(4) . . ?
C2 N2 C5 125.6(4) . . ?
C1 N1 C3 109.1(3) . . ?
N2 C1 N1 107.6(3) . . ?
N2 C1 C4 127.6(3) . . ?
N1 C1 C4 124.8(4) . . ?
C3 C2 N2 107.7(4) . . ?
C2 C3 N1 106.2(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.3041(10) . ?
Pd1 Cl1 2.3041(10) 3_556 ?
Pd1 Cl2 2.3090(11) 3_556 ?
Pd1 Cl2 2.3091(11) . ?
N2 C1 1.297(5) . ?
N2 C2 1.365(6) . ?
N2 C5 1.478(5) . ?
N1 C1 1.334(5) . ?
N1 C3 1.369(5) . ?
C1 C4 1.497(5) . ?
C2 C3 1.328(7) . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C2 C3 N1 0.1(5) . . . . ?
C1 N2 C2 C3 -0.5(5) . . . . ?
C1 N1 C3 C2 0.4(4) . . . . ?
C2 N2 C1 N1 0.7(4) . . . . ?
C2 N2 C1 C4 179.9(3) . . . . ?
C3 N1 C1 N2 -0.7(4) . . . . ?
C3 N1 C1 C4 -179.9(3) . . . . ?
C5 N2 C1 N1 -179.1(3) . . . . ?
C5 N2 C1 C4 0.1(6) . . . . ?
C5 N2 C2 C3 179.3(3) . . . . ?
