#------------------------------------------------------------------------------
#$Date: 2021-11-12 01:01:37 +0100 (vie 12 de nov de 2021) $
#$Revision: 270607 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/87/7708794.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_7708794
loop_
_publ_author_name
'Maliszewska, Hanna K.'
'Arnau del Valle, Carla'
'Xia, Ying'
'Marín, María J.'
'Waller, Zoë A. E.'
'Muñoz, María Paz'
_publ_section_title
;
 Precious metal complexes of bis(pyridyl)allenes: synthesis and catalytic
 and medicinal applications
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02929K
_journal_year                    2021
_chemical_formula_moiety         'C25 H26 Cl2 N2 Pd'
_chemical_formula_sum            'C25 H26 Cl2 N2 Pd'
_chemical_formula_weight         531.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-02
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-07-06 deposited with the CCDC.	2021-10-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.017(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3560(3)
_cell_length_b                   14.1423(4)
_cell_length_c                   17.5530(5)
_cell_measurement_reflns_used    21971
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1750
_cell_measurement_theta_min      2.2200
_cell_volume                     2262.85(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.799
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -77.00  11.00   0.50   11.71    --   -4.50 -58.00 -44.00  176
  2  ω      0.00  26.00   0.50   11.71    --   -4.50 -99.00   0.00   52
  3  ω    -21.00   5.00   0.50   11.71    --   -4.50 -77.00  60.00   52
  4  ω      2.00  28.00   0.50   11.71    --   -4.50 -99.00 120.00   52
  5  ω    -20.00  68.00   0.50   11.71    --   -4.50  58.00  97.00  176
  6  ω    -10.00  47.00   0.50   11.71    --    4.11  57.00 120.00  114
  7  ω      2.00  28.00   0.50   11.71    --    4.11 -99.00-150.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0258246000
_diffrn_orient_matrix_UB_12      -0.0309322000
_diffrn_orient_matrix_UB_13      -0.0257671000
_diffrn_orient_matrix_UB_21      -0.0728686000
_diffrn_orient_matrix_UB_22      -0.0154838000
_diffrn_orient_matrix_UB_23      -0.0156604000
_diffrn_orient_matrix_UB_31      -0.0089089000
_diffrn_orient_matrix_UB_32      0.0363229000
_diffrn_orient_matrix_UB_33      -0.0284765000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.799
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26885
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         2.234
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.071
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55327
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.68a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1080
_exptl_crystal_recrystallization_method
'vapour diffusion of dichloromethane/MeOH solution and n-Hex at 4 °C'
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.715
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         5767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0210P)²+2.4440P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0567
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5379
_reflns_number_total             5767
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt02929k2.cif
_cod_data_source_block           hm_233b_2
_cod_database_code               7708794
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C100 H104 Cl8 N8 Pd4 '
_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   0.980
_shelx_estimated_absorpt_t_min   0.718
_diffrn_oxdiff_digest_frames
;
019446f0bfe512f9b8df72e988ff815421000258f1f
;
_diffrn_oxdiff_digest_hkl
;
019fc68e755b3772f4203a70db6594ba45e637
;
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00D(H00D), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00N(H00N), C00P(H00P), C00R(H00S), C00T(H00W)
2.b Idealised Me refined as rotating group:
 C00M(H00A,H00C,H00E), C00O(H00F,H00L,H00M), C00Q(H00O,H00Q,H00R), C00S(H00T,
 H00U,H00V), C00U(H00X,H00Y,H)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.640
_oxdiff_exptl_absorpt_empirical_full_min 0.515
loop_
_space_group_symop_operation_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_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
Pd01 Pd 0.23589(2) 0.26030(2) 0.45262(2) 0.01033(4) Uani 1 1 d . . . . .
Cl02 Cl -0.00098(5) 0.27419(3) 0.47280(2) 0.01491(8) Uani 1 1 d . . . . .
Cl03 Cl 0.45436(5) 0.23306(3) 0.41466(3) 0.01711(9) Uani 1 1 d . . . . .
N004 N 0.25032(16) 0.12873(10) 0.49954(8) 0.0124(3) Uani 1 1 d . . . . .
N005 N 0.26346(16) 0.40353(10) 0.44580(8) 0.0121(3) Uani 1 1 d . . . . .
C006 C 0.29686(18) 0.44507(12) 0.51805(10) 0.0121(3) Uani 1 1 d . . . . .
C007 C 0.34975(18) 0.29868(12) 0.59236(9) 0.0122(3) Uani 1 1 d . . . . .
C008 C 0.34136(19) 0.12590(12) 0.57181(10) 0.0124(3) Uani 1 1 d . . . . .
C009 C 0.41219(19) 0.21482(12) 0.60723(9) 0.0124(3) Uani 1 1 d . . . . .
C00A C 0.29301(18) 0.38463(11) 0.58769(9) 0.0114(3) Uani 1 1 d . . . . .
C00B C 0.3024(2) 0.55015(13) 0.38646(11) 0.0172(3) Uani 1 1 d . . . . .
H00B H 0.303231 0.584860 0.341552 0.021 Uiso 1 1 calc R . . . .
C00C C 0.56143(19) 0.20906(12) 0.66104(10) 0.0127(3) Uani 1 1 d . . . . .
C00D C 0.8228(2) 0.18341(13) 0.68071(11) 0.0178(4) Uani 1 1 d . . . . .
H00D H 0.903756 0.167253 0.660924 0.021 Uiso 1 1 calc R . . . .
C00E C 0.1779(2) 0.05039(12) 0.46739(10) 0.0153(3) Uani 1 1 d . . . . .
C00F C 0.21711(19) 0.41975(12) 0.65224(10) 0.0129(3) Uani 1 1 d . . . . .
C00G C 0.6826(2) 0.18166(12) 0.63216(10) 0.0156(3) Uani 1 1 d . . . . .
H00G H 0.669787 0.162229 0.580445 0.019 Uiso 1 1 calc R . . . .
C00H C 0.33391(19) 0.54040(12) 0.52510(10) 0.0146(3) Uani 1 1 d . . . . .
H00H H 0.357138 0.568657 0.574183 0.018 Uiso 1 1 calc R . . . .
C00I C 0.3362(2) 0.59336(13) 0.45879(11) 0.0182(4) Uani 1 1 d . . . . .
H00I H 0.360224 0.657246 0.463073 0.022 Uiso 1 1 calc R . . . .
C00J C 0.7212(2) 0.23351(13) 0.78827(11) 0.0182(4) Uani 1 1 d . . . . .
H00J H 0.733762 0.248980 0.840859 0.022 Uiso 1 1 calc R . . . .
C00K C 0.5813(2) 0.23482(12) 0.73970(10) 0.0154(3) Uani 1 1 d . . . . .
H00K H 0.501156 0.252794 0.759490 0.019 Uiso 1 1 calc R . . . .
C00L C 0.26712(19) 0.45422(12) 0.38100(10) 0.0140(3) Uani 1 1 d . . . . .
C00M C 0.3314(2) 0.46955(13) 0.71699(10) 0.0169(3) Uani 1 1 d . . . . .
H00A H 0.408398 0.425916 0.738806 0.025 Uiso 1 1 calc GR . . . .
H00C H 0.284938 0.491060 0.757314 0.025 Uiso 1 1 calc GR . . . .
H00E H 0.372083 0.522642 0.695107 0.025 Uiso 1 1 calc GR . . . .
C00N C 0.8415(2) 0.20936(13) 0.75887(12) 0.0199(4) Uani 1 1 d . . . . .
H00N H 0.934993 0.210447 0.791309 0.024 Uiso 1 1 calc R . . . .
C00O C 0.1545(2) 0.33385(13) 0.68770(11) 0.0184(4) Uani 1 1 d . . . . .
H00F H 0.088463 0.299954 0.647064 0.028 Uiso 1 1 calc GR . . . .
H00L H 0.102608 0.355119 0.725879 0.028 Uiso 1 1 calc GR . . . .
H00M H 0.233312 0.292931 0.712266 0.028 Uiso 1 1 calc GR . . . .
C00P C 0.3669(2) 0.04096(12) 0.61261(11) 0.0163(3) Uani 1 1 d . . . . .
H00P H 0.432758 0.038300 0.660917 0.020 Uiso 1 1 calc R . . . .
C00Q C 0.0891(2) 0.48662(13) 0.61861(11) 0.0183(4) Uani 1 1 d . . . . .
H00O H 0.125976 0.542347 0.598372 0.027 Uiso 1 1 calc GR . . . .
H00Q H 0.040328 0.504104 0.659144 0.027 Uiso 1 1 calc GR . . . .
H00R H 0.020910 0.455220 0.577292 0.027 Uiso 1 1 calc GR . . . .
C00R C 0.1964(2) -0.03445(13) 0.50802(11) 0.0177(3) Uani 1 1 d . . . . .
H00S H 0.143940 -0.087655 0.486619 0.021 Uiso 1 1 calc R . . . .
C00S C 0.2329(2) 0.40412(14) 0.30362(10) 0.0192(4) Uani 1 1 d . . . . .
H00T H 0.319096 0.371998 0.296098 0.029 Uiso 1 1 calc GR . . . .
H00U H 0.201828 0.449354 0.262442 0.029 Uiso 1 1 calc GR . . . .
H00V H 0.156001 0.358959 0.302828 0.029 Uiso 1 1 calc GR . . . .
C00T C 0.2925(2) -0.04008(12) 0.58024(11) 0.0188(4) Uani 1 1 d . . . . .
H00W H 0.307464 -0.097312 0.606952 0.023 Uiso 1 1 calc R . . . .
C00U C 0.0835(2) 0.06006(14) 0.38655(11) 0.0206(4) Uani 1 1 d . . . . .
H00X H 0.016886 0.111946 0.385238 0.031 Uiso 1 1 calc GR . . . .
H00Y H 0.028905 0.002791 0.372431 0.031 Uiso 1 1 calc GR . . . .
H H 0.144430 0.071617 0.350217 0.031 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
Cl02 Pd01 C007 92.41(4) . . ?
Cl03 Pd01 Cl02 170.825(16) . . ?
Cl03 Pd01 C007 96.28(4) . . ?
N004 Pd01 Cl02 89.67(4) . . ?
N004 Pd01 Cl03 88.97(4) . . ?
N004 Pd01 N005 159.00(6) . . ?
N004 Pd01 C007 80.00(6) . . ?
N005 Pd01 Cl02 93.56(4) . . ?
N005 Pd01 Cl03 90.96(4) . . ?
N005 Pd01 C007 79.13(6) . . ?
C008 N004 Pd01 112.11(11) . . ?
C00E N004 Pd01 126.91(12) . . ?
C00E N004 C008 120.95(15) . . ?
C006 N005 Pd01 112.07(11) . . ?
C00L N005 Pd01 126.94(12) . . ?
C00L N005 C006 120.56(15) . . ?
N005 C006 C00A 117.94(14) . . ?
N005 C006 C00H 119.93(16) . . ?
C00H C006 C00A 122.12(15) . . ?
C009 C007 Pd01 94.04(11) . . ?
C00A C007 Pd01 93.57(11) . . ?
C00A C007 C009 172.31(17) . . ?
N004 C008 C009 119.37(14) . . ?
N004 C008 C00P 120.28(16) . . ?
C00P C008 C009 120.34(15) . . ?
C007 C009 C008 122.65(15) . . ?
C007 C009 C00C 118.68(15) . . ?
C008 C009 C00C 118.67(14) . . ?
C006 C00A C00F 120.87(14) . . ?
C007 C00A C006 119.48(16) . . ?
C007 C00A C00F 119.58(15) . . ?
C00I C00B C00L 119.70(17) . . ?
C00G C00C C009 120.17(15) . . ?
C00G C00C C00K 119.47(16) . . ?
C00K C00C C009 120.31(16) . . ?
C00N C00D C00G 119.95(18) . . ?
N004 C00E C00R 120.07(16) . . ?
N004 C00E C00U 116.92(16) . . ?
C00R C00E C00U 122.98(16) . . ?
C00M C00F C00A 109.21(14) . . ?
C00O C00F C00A 108.78(14) . . ?
C00O C00F C00M 109.02(14) . . ?
C00Q C00F C00A 111.28(14) . . ?
C00Q C00F C00M 110.67(14) . . ?
C00Q C00F C00O 107.83(15) . . ?
C00D C00G C00C 120.13(17) . . ?
C00I C00H C006 119.94(17) . . ?
C00B C00I C00H 119.27(16) . . ?
C00N C00J C00K 120.46(17) . . ?
C00J C00K C00C 119.91(17) . . ?
N005 C00L C00B 120.59(16) . . ?
N005 C00L C00S 118.07(15) . . ?
C00B C00L C00S 121.35(16) . . ?
C00J C00N C00D 120.02(17) . . ?
C008 C00P C00T 119.22(16) . . ?
C00T C00R C00E 120.12(17) . . ?
C00R C00T C00P 119.25(16) . . ?
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
Pd01 Cl02 2.3300(4) . ?
Pd01 Cl03 2.3203(5) . ?
Pd01 N004 2.0269(14) . ?
Pd01 N005 2.0489(14) . ?
Pd01 C007 2.5038(16) . ?
N004 C008 1.360(2) . ?
N004 C00E 1.354(2) . ?
N005 C006 1.368(2) . ?
N005 C00L 1.351(2) . ?
C006 C00A 1.499(2) . ?
C006 C00H 1.391(2) . ?
C007 C009 1.322(2) . ?
C007 C00A 1.321(2) . ?
C008 C009 1.490(2) . ?
C008 C00P 1.391(2) . ?
C009 C00C 1.501(2) . ?
C00A C00F 1.548(2) . ?
C00B C00I 1.380(3) . ?
C00B C00L 1.395(2) . ?
C00C C00G 1.397(3) . ?
C00C C00K 1.399(2) . ?
C00D C00G 1.394(2) . ?
C00D C00N 1.393(3) . ?
C00E C00R 1.387(3) . ?
C00E C00U 1.499(2) . ?
C00F C00M 1.544(2) . ?
C00F C00O 1.540(2) . ?
C00F C00Q 1.536(2) . ?
C00H C00I 1.388(2) . ?
C00J C00K 1.392(3) . ?
C00J C00N 1.383(3) . ?
C00L C00S 1.501(2) . ?
C00P C00T 1.394(3) . ?
C00R C00T 1.382(3) . ?
