#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:59:52 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232983 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/84/4348479.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_4348479
loop_
_publ_author_name
'Charette, Bronte J.'
'Ritch, Jamie S.'
_publ_section_title
;
 A Selenium-Containing Diarylamido Pincer Ligand: Synthesis and
 Coordination Chemistry with Group 10 Metals.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6344
_journal_page_last               6350
_journal_paper_doi               10.1021/acs.inorgchem.6b01203
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C16 H18 Cl N Pd Se2'
_chemical_formula_sum            'C16 H18 Cl N Pd Se2'
_chemical_formula_weight         524.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.1590(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1538(5)
_cell_length_b                   9.5448(3)
_cell_length_c                   12.7299(4)
_cell_measurement_reflns_used    7721
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      32.03
_cell_measurement_theta_min      2.58
_cell_volume                     1717.12(10)
_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      295.09
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_unetI/netI     0.0150
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14295
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         3.371
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.468
_exptl_absorpt_correction_T_max  0.8625
_exptl_absorpt_correction_T_min  0.6661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0773 before and 0.0459 after correction.
The Ratio of minimum to maximum transmission is 0.7723.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.027
_exptl_crystal_description       prism
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1512
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0232
_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)+(0.0179P)²+6.5112P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0509
_refine_ls_wR_factor_ref         0.0605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1288
_reflns_number_total             1512
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01203_si_002.cif
_cod_data_source_block           Compound3-Pd
_cod_database_code               4348479
_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.
;
_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:
 C2(H2), C5(H5), C3(H3)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C7(H7A,H7B,H7C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Pd1 Pd 0.5000 0.15774(4) 0.2500 0.03453(14) Uani 1 2 d S T P
Se1 Se 0.53291(3) 0.17425(4) 0.44741(3) 0.03819(14) Uani 1 1 d . . .
Cl1 Cl 0.5000 -0.08403(15) 0.2500 0.0731(6) Uani 1 2 d S T P
N1 N 0.5000 0.3672(4) 0.2500 0.0332(10) Uani 1 2 d S T P
C1 C 0.5509(3) 0.4364(3) 0.3498(3) 0.0279(8) Uani 1 1 d . . .
C6 C 0.5743(3) 0.3654(4) 0.4531(3) 0.0317(8) Uani 1 1 d . . .
C2 C 0.5864(3) 0.5733(4) 0.3573(3) 0.0326(8) Uani 1 1 d . . .
H2 H 0.5760 0.6242 0.2916 0.039 Uiso 1 1 calc R . .
C5 C 0.6235(3) 0.4279(4) 0.5550(3) 0.0366(9) Uani 1 1 d . . .
H5 H 0.6351 0.3772 0.6211 0.044 Uiso 1 1 calc R . .
C3 C 0.6365(3) 0.6344(4) 0.4599(3) 0.0358(8) Uani 1 1 d . . .
H3 H 0.6578 0.7259 0.4610 0.043 Uiso 1 1 calc R . .
C4 C 0.6562(3) 0.5644(4) 0.5616(3) 0.0389(9) Uani 1 1 d . . .
C8 C 0.6546(3) 0.0810(5) 0.5094(4) 0.0613(13) Uani 1 1 d . . .
H8A H 0.6991 0.1267 0.4830 0.092 Uiso 1 1 calc GR . .
H8B H 0.6478 -0.0152 0.4857 0.092 Uiso 1 1 calc GR . .
H8C H 0.6770 0.0853 0.5901 0.092 Uiso 1 1 calc GR . .
C7 C 0.7121(3) 0.6323(6) 0.6730(4) 0.0571(12) Uani 1 1 d . . .
H7A H 0.6914 0.5957 0.7305 0.086 Uiso 1 1 calc GR . .
H7B H 0.7021 0.7318 0.6672 0.086 Uiso 1 1 calc GR . .
H7C H 0.7782 0.6127 0.6920 0.086 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'
Se Se -0.0929 2.2259 '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
Se1 Pd1 Se1 172.42(2) 2_655 .
Cl1 Pd1 Se1 93.788(12) . 2_655
Cl1 Pd1 Se1 93.789(12) . .
N1 Pd1 Se1 86.212(12) . 2_655
N1 Pd1 Se1 86.211(12) . .
N1 Pd1 Cl1 180.0 . .
C6 Se1 Pd1 92.49(11) . .
C6 Se1 C8 99.83(19) . .
C8 Se1 Pd1 101.82(16) . .
C1 N1 Pd1 118.3(2) . .
C1 N1 Pd1 118.3(2) 2_655 .
C1 N1 C1 123.4(4) . 2_655
N1 C1 C6 119.7(3) . .
N1 C1 C2 125.2(3) . .
C2 C1 C6 115.1(3) . .
C1 C6 Se1 117.0(3) . .
C5 C6 Se1 120.3(3) . .
C5 C6 C1 122.7(3) . .
C1 C2 H2 119.2 . .
C3 C2 C1 121.6(4) . .
C3 C2 H2 119.2 . .
C6 C5 H5 119.2 . .
C6 C5 C4 121.6(4) . .
C4 C5 H5 119.2 . .
C2 C3 H3 118.7 . .
C2 C3 C4 122.6(4) . .
C4 C3 H3 118.7 . .
C5 C4 C3 116.3(4) . .
C5 C4 C7 121.8(4) . .
C3 C4 C7 121.8(4) . .
Se1 C8 H8A 109.5 . .
Se1 C8 H8B 109.5 . .
Se1 C8 H8C 109.5 . .
H8A C8 H8B 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
C4 C7 H7A 109.5 . .
C4 C7 H7B 109.5 . .
C4 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 Se1 2.3841(4) .
Pd1 Se1 2.3841(4) 2_655
Pd1 Cl1 2.3077(15) .
Pd1 N1 1.999(4) .
Se1 C6 1.923(4) .
Se1 C8 1.940(4) .
N1 C1 1.392(4) .
N1 C1 1.392(4) 2_655
C1 C6 1.405(5) .
C1 C2 1.404(5) .
C6 C5 1.378(5) .
C2 H2 0.9300 .
C2 C3 1.380(5) .
C5 H5 0.9300 .
C5 C4 1.386(6) .
C3 H3 0.9300 .
C3 C4 1.390(6) .
C4 C7 1.510(6) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
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
Pd1 N1 C1 C6 -20.5(4) .
Pd1 N1 C1 C2 156.1(3) .
Se1 C6 C5 C4 178.5(3) .
N1 C1 C6 Se1 -0.1(4) .
N1 C1 C6 C5 -179.2(3) .
N1 C1 C2 C3 -179.9(3) .
C1 N1 C1 C6 159.5(4) 2_655
C1 N1 C1 C2 -23.9(3) 2_655
C1 C6 C5 C4 -2.4(6) .
C1 C2 C3 C4 1.0(6) .
C6 C1 C2 C3 -3.1(5) .
C6 C5 C4 C3 0.1(5) .
C6 C5 C4 C7 -178.6(4) .
C2 C1 C6 Se1 -177.0(3) .
C2 C1 C6 C5 3.8(5) .
C2 C3 C4 C5 0.6(6) .
C2 C3 C4 C7 179.3(4) .
