#------------------------------------------------------------------------------
#$Date: 2015-08-05 21:19:17 +0300 (Wed, 05 Aug 2015) $
#$Revision: 152814 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/34/4343488.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_4343488
loop_
_publ_author_name
'Barnett, Brandon R.'
'Labios, Liezel A.'
'Moore, Curtis E.'
'England, Jason'
'Rheingold, Arnold L.'
'Wieghardt, Karl'
'Figueroa, Joshua S.'
_publ_section_title
;
 Solution Dynamics of Redox Noninnocent Nitrosoarene Ligands: Mapping the
 Electronic Criteria for the Formation of Persistent Metal-Coordinated
 Nitroxide Radicals.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7110
_journal_page_last               7121
_journal_paper_doi               10.1021/acs.inorgchem.5b01252
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C76 H88 N4 O2 Pd, 2(C4 H10 O)'
_chemical_formula_sum            'C84 H108 N4 O4 Pd'
_chemical_formula_weight         1344.14
_chemical_name_common            Pd(k1-N-p-MeArNO)2(CNArDipp2)2
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 113.135(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.973(2)
_cell_length_b                   17.461(3)
_cell_length_c                   16.912(3)
_cell_measurement_reflns_used    6747
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.33
_cell_volume                     3794.4(11)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.931
_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  0.0857
_diffrn_reflns_av_unetI/netI     0.0773
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37917
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.276
_diffrn_reflns_theta_min         1.753
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.295
_exptl_absorpt_correction_T_max  0.9711
_exptl_absorpt_correction_T_min  0.9406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.424
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         8777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0518
_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)+(0.0551P)²+2.6013P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1332
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6121
_reflns_number_total             8777
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01252_si_002.cif
_cod_data_source_block           jfig373
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4343481--4343500.cif.
;
_cod_original_cell_volume        3794.4(10)
_cod_database_code               4343488
_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.
;
_shelxl_version_number           2014/6
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
C1 C 0.0491(2) 0.08491(16) 0.94535(19) 0.0210(6) Uani 1 1 d . . .
C2 C 0.1175(2) 0.18557(15) 0.87032(18) 0.0187(6) Uani 1 1 d . . .
C3 C 0.2150(2) 0.17090(15) 0.86992(18) 0.0195(6) Uani 1 1 d . . .
C4 C 0.2534(2) 0.22348(16) 0.82721(19) 0.0226(6) Uani 1 1 d . . .
H4 H 0.3197 0.2152 0.8253 0.027 Uiso 1 1 calc R U .
C5 C 0.1960(2) 0.28751(17) 0.78758(19) 0.0228(6) Uani 1 1 d . . .
H5 H 0.2230 0.3224 0.7584 0.027 Uiso 1 1 calc R U .
C6 C 0.0989(2) 0.30118(16) 0.79011(19) 0.0223(6) Uani 1 1 d . . .
H6 H 0.0606 0.3455 0.7630 0.027 Uiso 1 1 calc R U .
C7 C 0.0574(2) 0.25052(16) 0.83205(18) 0.0198(6) Uani 1 1 d . . .
C8 C 0.2757(2) 0.10158(16) 0.9131(2) 0.0217(6) Uani 1 1 d . . .
C9 C 0.3439(2) 0.10507(17) 1.0005(2) 0.0237(6) Uani 1 1 d . . .
C10 C 0.3958(3) 0.03871(19) 1.0399(2) 0.0308(7) Uani 1 1 d . . .
H10 H 0.4404 0.0398 1.0992 0.037 Uiso 1 1 calc R U .
C11 C 0.3834(3) -0.02893(19) 0.9941(2) 0.0325(8) Uani 1 1 d . . .
H11 H 0.4207 -0.0734 1.0218 0.039 Uiso 1 1 calc R U .
C12 C 0.3175(3) -0.03194(18) 0.9090(2) 0.0314(7) Uani 1 1 d . . .
H12 H 0.3095 -0.0788 0.8784 0.038 Uiso 1 1 calc R U .
C13 C 0.2616(3) 0.03284(18) 0.8663(2) 0.0275(7) Uani 1 1 d . . .
C14 C -0.0452(2) 0.26652(16) 0.83713(19) 0.0225(6) Uani 1 1 d . . .
C15 C -0.1384(2) 0.25161(17) 0.7656(2) 0.0261(7) Uani 1 1 d . . .
C16 C -0.2323(3) 0.2706(2) 0.7711(2) 0.0342(8) Uani 1 1 d . . .
H16 H -0.2959 0.2597 0.7240 0.041 Uiso 1 1 calc R U .
C17 C -0.2344(3) 0.3051(2) 0.8442(2) 0.0377(9) Uani 1 1 d . . .
H17 H -0.2991 0.3186 0.8465 0.045 Uiso 1 1 calc R U .
C18 C -0.1433(3) 0.3197(2) 0.9132(2) 0.0370(8) Uani 1 1 d . . .
H18 H -0.1459 0.3433 0.9629 0.044 Uiso 1 1 calc R U .
C19 C -0.0468(3) 0.30057(18) 0.9120(2) 0.0274(7) Uani 1 1 d . . .
C20 C 0.1900(3) 0.0267(2) 0.7717(2) 0.0424(9) Uani 1 1 d . . .
H20 H 0.1577 0.0782 0.7527 0.051 Uiso 1 1 calc R U .
C21 C 0.2503(4) 0.0066(2) 0.7178(3) 0.0632(13) Uani 1 1 d . . .
H21A H 0.3014 0.0469 0.7235 0.095 Uiso 1 1 calc R U .
H21B H 0.2023 0.0021 0.6574 0.095 Uiso 1 1 calc R U .
H21C H 0.2864 -0.0422 0.7375 0.095 Uiso 1 1 calc R U .
C22 C 0.1015(3) -0.0308(2) 0.7582(3) 0.0513(11) Uani 1 1 d . . .
H22A H 0.1305 -0.0826 0.7720 0.077 Uiso 1 1 calc R U .
H22B H 0.0520 -0.0291 0.6981 0.077 Uiso 1 1 calc R U .
H22C H 0.0657 -0.0175 0.7958 0.077 Uiso 1 1 calc R U .
C23 C 0.3627(2) 0.17963(18) 1.0509(2) 0.0272(7) Uani 1 1 d . . .
H23 H 0.3219 0.2207 1.0106 0.033 Uiso 1 1 calc R U .
C24 C 0.4777(3) 0.2021(2) 1.0848(3) 0.0469(10) Uani 1 1 d . . .
H24A H 0.5192 0.1641 1.1269 0.070 Uiso 1 1 calc R U .
H24B H 0.4870 0.2526 1.1123 0.070 Uiso 1 1 calc R U .
H24C H 0.5004 0.2041 1.0369 0.070 Uiso 1 1 calc R U .
C25 C 0.3250(3) 0.1752(2) 1.1246(2) 0.0415(9) Uani 1 1 d . . .
H25A H 0.2514 0.1604 1.1016 0.062 Uiso 1 1 calc R U .
H25B H 0.3334 0.2253 1.1526 0.062 Uiso 1 1 calc R U .
H25C H 0.3661 0.1369 1.1666 0.062 Uiso 1 1 calc R U .
C26 C 0.0528(3) 0.3202(2) 0.9882(2) 0.0338(8) Uani 1 1 d . . .
H26 H 0.1119 0.2955 0.9786 0.041 Uiso 1 1 calc R U .
C27 C 0.0538(4) 0.2906(3) 1.0732(3) 0.0667(14) Uani 1 1 d . . .
H27A H 0.0032 0.3193 1.0884 0.100 Uiso 1 1 calc R U .
H27B H 0.1235 0.2972 1.1183 0.100 Uiso 1 1 calc R U .
H27C H 0.0353 0.2361 1.0675 0.100 Uiso 1 1 calc R U .
C28 C 0.0700(4) 0.4058(3) 0.9921(3) 0.0821(18) Uani 1 1 d . . .
H28A H 0.0722 0.4234 0.9378 0.123 Uiso 1 1 calc R U .
H28B H 0.1360 0.4180 1.0396 0.123 Uiso 1 1 calc R U .
H28C H 0.0128 0.4315 1.0013 0.123 Uiso 1 1 calc R U .
C29 C -0.1376(3) 0.21522(18) 0.6842(2) 0.0292(7) Uani 1 1 d . . .
H29 H -0.0655 0.2208 0.6860 0.035 Uiso 1 1 calc R U .
C30 C -0.1608(4) 0.1297(2) 0.6818(3) 0.0563(12) Uani 1 1 d . . .
H30A H -0.1113 0.1054 0.7341 0.084 Uiso 1 1 calc R U .
H30B H -0.1543 0.1067 0.6313 0.084 Uiso 1 1 calc R U .
H30C H -0.2318 0.1222 0.6785 0.084 Uiso 1 1 calc R U .
C31 C -0.2110(4) 0.2553(3) 0.6032(2) 0.0578(12) Uani 1 1 d . . .
H31A H -0.2828 0.2497 0.5986 0.087 Uiso 1 1 calc R U .
H31B H -0.2043 0.2322 0.5528 0.087 Uiso 1 1 calc R U .
H31C H -0.1931 0.3098 0.6061 0.087 Uiso 1 1 calc R U .
C32 C 0.2114(2) -0.02517(17) 1.1432(2) 0.0244(7) Uani 1 1 d . . .
C33 C 0.2198(2) -0.08758(17) 1.0942(2) 0.0270(7) Uani 1 1 d . . .
H33 H 0.1633 -0.1007 1.0423 0.032 Uiso 1 1 calc R U .
C34 C 0.3106(3) -0.12985(18) 1.1220(2) 0.0326(8) Uani 1 1 d . . .
H34 H 0.3153 -0.1727 1.0891 0.039 Uiso 1 1 calc R U .
C35 C 0.3956(3) -0.1112(2) 1.1972(2) 0.0346(8) Uani 1 1 d . . .
C36 C 0.3859(3) -0.0502(2) 1.2462(2) 0.0370(8) Uani 1 1 d . . .
H36 H 0.4423 -0.0377 1.2984 0.044 Uiso 1 1 calc R U .
C37 C 0.2952(2) -0.00708(19) 1.2203(2) 0.0317(7) Uani 1 1 d . . .
H37 H 0.2900 0.0345 1.2545 0.038 Uiso 1 1 calc R U .
C38 C 0.4970(3) -0.1553(2) 1.2231(3) 0.0530(11) Uani 1 1 d . . .
H38A H 0.5276 -0.1463 1.1808 0.080 Uiso 1 1 calc R U .
H38B H 0.4834 -0.2101 1.2254 0.080 Uiso 1 1 calc R U .
H38C H 0.5454 -0.1379 1.2798 0.080 Uiso 1 1 calc R U .
C1S C 0.3297(4) 0.4772(3) -0.0115(3) 0.0675(14) Uani 1 1 d . . .
H1SA H 0.3409 0.4837 -0.0654 0.081 Uiso 1 1 calc R U .
H1SB H 0.2602 0.4981 -0.0205 0.081 Uiso 1 1 calc R U .
C2S C 0.3353(4) 0.3937(3) 0.0121(3) 0.0755(15) Uani 1 1 d . . .
H2SA H 0.4031 0.3730 0.0183 0.113 Uiso 1 1 calc R U .
H2SB H 0.2799 0.3657 -0.0332 0.113 Uiso 1 1 calc R U .
H2SC H 0.3267 0.3881 0.0666 0.113 Uiso 1 1 calc R U .
C3S C 0.4094(4) 0.5982(3) 0.0418(3) 0.0637(13) Uani 1 1 d . . .
H3SA H 0.3409 0.6201 0.0338 0.076 Uiso 1 1 calc R U .
H3SB H 0.4208 0.6067 -0.0117 0.076 Uiso 1 1 calc R U .
C4S C 0.4930(4) 0.6374(3) 0.1150(3) 0.0771(16) Uani 1 1 d . . .
H4SA H 0.4861 0.6243 0.1689 0.116 Uiso 1 1 calc R U .
H4SB H 0.4865 0.6929 0.1063 0.116 Uiso 1 1 calc R U .
H4SC H 0.5612 0.6207 0.1179 0.116 Uiso 1 1 calc R U .
N1 N 0.1210(2) 0.01900(13) 1.11407(16) 0.0227(5) Uani 1 1 d . . .
N2 N 0.07694(18) 0.13207(13) 0.91180(15) 0.0184(5) Uani 1 1 d . . .
O1 O 0.11221(18) 0.07529(13) 1.15804(15) 0.0347(6) Uani 1 1 d . . .
O1S O 0.4097(3) 0.51739(19) 0.0583(2) 0.0698(9) Uani 1 1 d . . .
Pd1 Pd 0.0000 0.0000 1.0000 0.01714(10) Uani 1 2 d S . P
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'
O O 0.0106 0.0060 '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
N2 C1 Pd1 177.8(3) . .
C3 C2 C7 123.8(3) . .
C3 C2 N2 117.8(2) . .
C7 C2 N2 118.5(3) . .
C2 C3 C4 117.2(3) . .
C2 C3 C8 121.1(2) . .
C4 C3 C8 121.6(3) . .
C5 C4 C3 120.8(3) . .
C4 C5 C6 120.6(3) . .
C5 C6 C7 120.7(3) . .
C6 C7 C2 116.8(3) . .
C6 C7 C14 120.7(3) . .
C2 C7 C14 122.4(2) . .
C13 C8 C9 120.9(3) . .
C13 C8 C3 119.2(3) . .
C9 C8 C3 119.8(3) . .
C10 C9 C8 118.5(3) . .
C10 C9 C23 120.1(3) . .
C8 C9 C23 121.4(3) . .
C11 C10 C9 121.0(3) . .
C12 C11 C10 120.3(3) . .
C11 C12 C13 121.2(3) . .
C12 C13 C8 118.1(3) . .
C12 C13 C20 119.2(3) . .
C8 C13 C20 122.7(3) . .
C19 C14 C15 120.9(3) . .
C19 C14 C7 119.0(3) . .
C15 C14 C7 119.9(3) . .
C16 C15 C14 118.5(3) . .
C16 C15 C29 120.1(3) . .
C14 C15 C29 121.4(3) . .
C17 C16 C15 120.9(3) . .
C18 C17 C16 120.2(3) . .
C17 C18 C19 121.5(3) . .
C18 C19 C14 118.1(3) . .
C18 C19 C26 120.2(3) . .
C14 C19 C26 121.7(3) . .
C21 C20 C13 111.1(3) . .
C21 C20 C22 111.4(3) . .
C13 C20 C22 111.1(3) . .
C9 C23 C24 110.8(3) . .
C9 C23 C25 111.9(3) . .
C24 C23 C25 110.7(3) . .
C28 C26 C19 109.7(3) . .
C28 C26 C27 110.7(4) . .
C19 C26 C27 113.0(3) . .
C15 C29 C31 112.4(3) . .
C15 C29 C30 110.9(3) . .
C31 C29 C30 111.4(3) . .
N1 C32 C33 119.7(3) . .
N1 C32 C37 120.9(3) . .
C33 C32 C37 119.4(3) . .
C34 C33 C32 119.6(3) . .
C33 C34 C35 121.7(3) . .
C36 C35 C34 118.4(3) . .
C36 C35 C38 121.0(3) . .
C34 C35 C38 120.6(3) . .
C37 C36 C35 121.2(3) . .
C36 C37 C32 119.8(3) . .
O1S C1S C2S 108.0(4) . .
O1S C3S C4S 110.4(4) . .
O1 N1 C32 120.3(3) . .
O1 N1 Pd1 116.58(19) . .
C32 N1 Pd1 123.1(2) . .
C1 N2 C2 175.2(3) . .
C3S O1S C1S 112.0(3) . .
C1 Pd1 C1 180.0 3_557 .
C1 Pd1 N1 89.47(11) 3_557 .
C1 Pd1 N1 90.53(11) . .
C1 Pd1 N1 90.53(11) 3_557 3_557
C1 Pd1 N1 89.47(11) . 3_557
N1 Pd1 N1 180.0 . 3_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.151(4) .
C1 Pd1 2.005(3) .
C2 C3 1.388(4) .
C2 C7 1.409(4) .
C2 N2 1.414(3) .
C3 C4 1.399(4) .
C3 C8 1.494(4) .
C4 C5 1.386(4) .
C5 C6 1.394(4) .
C6 C7 1.395(4) .
C7 C14 1.496(4) .
C8 C13 1.409(4) .
C8 C9 1.410(4) .
C9 C10 1.391(4) .
C9 C23 1.522(4) .
C10 C11 1.386(5) .
C11 C12 1.372(5) .
C12 C13 1.403(5) .
C13 C20 1.520(5) .
C14 C19 1.407(4) .
C14 C15 1.410(4) .
C15 C16 1.392(4) .
C15 C29 1.520(4) .
C16 C17 1.386(5) .
C17 C18 1.371(5) .
C18 C19 1.396(5) .
C19 C26 1.518(5) .
C20 C21 1.506(6) .
C20 C22 1.540(5) .
C23 C24 1.529(5) .
C23 C25 1.533(5) .
C26 C28 1.512(5) .
C26 C27 1.522(5) .
C29 C31 1.521(5) .
C29 C30 1.525(5) .
C32 N1 1.394(4) .
C32 C33 1.401(4) .
C32 C37 1.404(4) .
C33 C34 1.382(4) .
C34 C35 1.395(5) .
C35 C36 1.389(5) .
C35 C38 1.518(5) .
C36 C37 1.388(5) .
C1S O1S 1.448(6) .
C1S C2S 1.506(6) .
C3S O1S 1.437(5) .
C3S C4S 1.493(6) .
N1 O1 1.267(3) .
N1 Pd1 2.032(3) .
Pd1 C1 2.005(3) 3_557
Pd1 N1 2.032(3) 3_557
