#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/83/1518358.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_1518358
loop_
_publ_author_name
'Hering, Florian'
'Nitsch, Jörn'
'Paul, Ursula'
'Steffen, Andreas'
'Bickelhaupt, F. Matthias'
'Radius, Udo'
_publ_section_title
;
 Bite-angle bending as a key for understanding group-10 metal reactivity
 of d10-[M(NHC)2] complexes with sterically modest NHC ligands
;
_journal_issue                   2
_journal_name_full               'Chem. Sci.'
_journal_page_first              1426
_journal_paper_doi               10.1039/C4SC02998D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_sum            'C18 H32 N4 Pd'
_chemical_formula_weight         410.87
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2014-09-19 deposited with the CCDC.
2014-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.210(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5147(10)
_cell_length_b                   8.7236(9)
_cell_length_c                   12.2763(13)
_cell_measurement_reflns_used    8460
_cell_measurement_temperature    168(2)
_cell_measurement_theta_max      26.15
_cell_measurement_theta_min      2.87
_cell_volume                     1012.98(18)
_computing_cell_refinement       'Saint-NT v. 7.23'
_computing_data_collection       'Smart-NT v. 5.63'
_computing_data_reduction        'Saint-NT v. 7.23'
_computing_molecular_graphics    'XP in ShelxTL-97'
_computing_publication_material  'XP in ShelxTL-97'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      168(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            18723
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.150
_diffrn_reflns_theta_min         2.153
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SadAbs-2008/1 (Bruker, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             428
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.397
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0211
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0349P)²+0.4323P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1775
_reflns_number_total             2018
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4sc02998d2.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
'Adding full bibliography for 1518358--1518359.cif.'
_cod_database_code               1518358
#BEGIN Tags that were not found in dictionaries:
_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   0.905
_shelx_estimated_absorpt_t_max   0.955
_shelxl_version_number           2013-2
#END Tags that were not found in dictionaries
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
Pd Pd 0.5000 0.0000 1.0000 0.01983(9) Uani 1 2 d S . P
C2 C 0.7379(2) 0.2637(2) 1.24625(17) 0.0288(4) Uani 1 1 d . . .
H2 H 0.8238 0.3060 1.2800 0.035 Uiso 1 1 calc R U .
N2 N 0.72061(16) 0.18071(19) 1.14981(13) 0.0239(3) Uani 1 1 d . . .
C3 C 0.6106(2) 0.2731(2) 1.28310(17) 0.0269(4) Uani 1 1 d . . .
H3 H 0.5885 0.3235 1.3477 0.032 Uiso 1 1 calc R U .
C4 C 0.3642(2) 0.1893(2) 1.21125(16) 0.0266(4) Uani 1 1 d . . .
H4 H 0.3265 0.1010 1.1651 0.032 Uiso 1 1 calc R U .
C5 C 0.2988(2) 0.3356(3) 1.16093(19) 0.0372(5) Uani 1 1 d . . .
H5A H 0.3241 0.3468 1.0861 0.056 Uiso 1 1 calc R U .
H5B H 0.3344 0.4239 1.2049 0.056 Uiso 1 1 calc R U .
H5C H 0.1957 0.3302 1.1594 0.056 Uiso 1 1 calc R U .
C6 C 0.3283(2) 0.1626(3) 1.32744(18) 0.0387(5) Uani 1 1 d . . .
H6A H 0.2258 0.1508 1.3268 0.058 Uiso 1 1 calc R U .
H6B H 0.3603 0.2503 1.3734 0.058 Uiso 1 1 calc R U .
H6C H 0.3756 0.0694 1.3570 0.058 Uiso 1 1 calc R U .
C7 C 0.8338(2) 0.1485(2) 1.08095(17) 0.0285(4) Uani 1 1 d . . .
H7 H 0.7928 0.0858 1.0171 0.034 Uiso 1 1 calc R U .
C9 C 0.9499(2) 0.0544(3) 1.1446(2) 0.0408(5) Uani 1 1 d . . .
H9A H 0.9108 -0.0436 1.1660 0.061 Uiso 1 1 calc R U .
H9B H 0.9877 0.1109 1.2103 0.061 Uiso 1 1 calc R U .
H9C H 1.0258 0.0355 1.0983 0.061 Uiso 1 1 calc R U .
C8 C 0.8892(2) 0.2971(3) 1.03690(19) 0.0403(5) Uani 1 1 d . . .
H8A H 0.9618 0.2739 0.9884 0.060 Uiso 1 1 calc R U .
H8B H 0.9303 0.3605 1.0981 0.060 Uiso 1 1 calc R U .
H8C H 0.8112 0.3527 0.9957 0.060 Uiso 1 1 calc R U .
C1 C 0.58365(19) 0.1355(2) 1.12420(15) 0.0213(4) Uani 1 1 d . . .
N1 N 0.51805(16) 0.19496(18) 1.20838(12) 0.0219(3) Uani 1 1 d . . .
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'
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
C1 Pd C1 180.0 3_657
C3 C2 N2 107.03(17) .
C3 C2 H2 126.5 .
N2 C2 H2 126.5 .
C1 N2 C2 111.78(16) .
C1 N2 C7 123.66(16) .
C2 N2 C7 124.54(16) .
C2 C3 N1 106.27(17) .
C2 C3 H3 126.9 .
N1 C3 H3 126.9 .
N1 C4 C6 110.71(16) .
N1 C4 C5 109.13(17) .
C6 C4 C5 112.70(18) .
N1 C4 H4 108.1 .
C6 C4 H4 108.1 .
C5 C4 H4 108.1 .
C4 C5 H5A 109.5 .
C4 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C4 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
C4 C6 H6A 109.5 .
C4 C6 H6B 109.5 .
H6A C6 H6B 109.5 .
C4 C6 H6C 109.5 .
H6A C6 H6C 109.5 .
H6B C6 H6C 109.5 .
N2 C7 C8 110.23(18) .
N2 C7 C9 110.18(17) .
C8 C7 C9 112.47(19) .
N2 C7 H7 107.9 .
C8 C7 H7 107.9 .
C9 C7 H7 107.9 .
C7 C9 H9A 109.5 .
C7 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C7 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
N2 C1 N1 102.64(15) .
N2 C1 Pd 129.07(14) .
N1 C1 Pd 128.12(13) .
C1 N1 C3 112.28(15) .
C1 N1 C4 122.92(15) .
C3 N1 C4 124.49(15) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd C1 2.0230(18) 3_657
Pd C1 2.0231(18) .
C2 C3 1.341(3) .
C2 N2 1.382(2) .
C2 H2 0.9500 .
N2 C1 1.365(2) .
N2 C7 1.467(2) .
C3 N1 1.381(2) .
C3 H3 0.9500 .
C4 N1 1.468(2) .
C4 C6 1.520(3) .
C4 C5 1.521(3) .
C4 H4 1.0000 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 C8 1.520(3) .
C7 C9 1.522(3) .
C7 H7 1.0000 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C1 N1 1.366(2) .
