Solution Dynamics of Redox Noninnocent Nitrosoarene Ligands: Mapping the Electronic Criteria for the Formation of Persistent Metal-Coordinated Nitroxide Radicals.
Barnett, Brandon R.; Labios, Liezel A.; Moore, Curtis E.; England, Jason; Rheingold, Arnold L.; Wieghardt, Karl; Figueroa, Joshua S.; Inorganic chemistry 54 (2015) 7110–7121; doi:10.1021/acs.inorgchem.5b01252

data_4343489
_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 H84 N4 O4 Pd'
_chemical_formula_sum            'C76 H84 N4 O4 Pd'
_chemical_formula_weight         1223.87
_chemical_name_common            Pd(k1-N-p-COHC6H4NO)2(CNArDipp2)2
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-08
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.702(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3005(9)
_cell_length_b                   17.1080(11)
_cell_length_c                   16.6238(11)
_cell_measurement_reflns_used    8530
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      2.73
_cell_volume                     3724.0(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_laue_measured_fraction_full 0.981
_diffrn_reflns_laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21167
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.375
_diffrn_reflns_theta_min         2.381
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_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            purple
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
SQUEEZE/PLATON located two sizeable solvent-accessible voids in the unit cell, 
however each is estimated to contain only 28 electrons. As removing this electon
density from the unit cell did not result in a change in the final R1 value upon
further refinement, these voids are assumed to be either empty or contain 
solvent molecules at low occupancy.
;
_refine_diff_density_max         1.099
_refine_diff_density_min         -1.162
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0822
_refine_ls_R_factor_gt           0.0559
_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/[\s^2^(Fo^2^)+(0.1021P)^2^+0.8457P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1662
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4791
_reflns_number_total             6685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01252_si_002.cif
_cod_data_source_block           jfig668
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_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_database_code               4343489
_shelxl_version_number           2014/6
_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. Uiso/Uaniso restraints and constraints
Uanis(C38) = Uanis(O2) = Uanis(O2B) = Uanis(C38B)
3. Others
 Fixed Sof: C38(0.65) H38(0.65) O2(0.65) O2B(0.35) C38B(0.35) H38B(0.35)
4.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C26(H26), C29(H29)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17),
 C18(H18), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C38B(H38B)
4.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              29041
_shelx_hkl_checksum              59415
_olex2_submission_special_instructions 'No special instructions were received'