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_4343497
_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         'C68 H78 F N3 O Pd, C6 H6'
_chemical_formula_sum            'C74 H84 F N3 O Pd'
_chemical_formula_weight         1156.84
_chemical_name_common            Pd(h2-N,O-p-FC6H4NO)(CNArDipp2)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-01
_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                 95.090(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0835(8)
_cell_length_b                   20.4568(8)
_cell_length_c                   21.9700(11)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      3.19
_cell_volume                     6304.7(5)
_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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_laue_measured_fraction_full 0.999
_diffrn_reflns_laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.403
_diffrn_reflns_theta_min         2.050
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.343
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_correction_T_min  0.9011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.219
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.443
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.10(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.304
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         10909
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.304
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0265P)^2^+53.9950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1707
_reflns_Friedel_coverage         0.998
_reflns_friedel_fraction_full    0.999
_reflns_friedel_fraction_max     0.995
_reflns_number_gt                10639
_reflns_number_total             10909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01252_si_002.cif
_cod_data_source_block           jfig724
_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               4343497
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.967
_shelx_estimated_absorpt_t_min   0.901
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.90(5) 0.10(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C33) = Uanis(C34)
Uanis(C38) = Uanis(C39)
Uanis(C28) = Uanis(C28B)
Uanis(C29) = Uanis(C29B) = Uanis(C27B)
Uanis(C50) = Uanis(C51)
4. Others
 Sof(C27B)=Sof(H27B)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=
 Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C21(H21), C24(H24), C27(H27), C27B(H27B), C30(H30), C51(H51), C54(H54),
 C57(H57), C60(H60)
5.b Me refined with riding coordinates:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C28B(H28D,H28E,H28F), C29B(H29D,
 H29E,H29F)
5.c Aromatic/amide H refined with riding coordinates:
 C1S(H1S), C2S(H2S), C3S(H3S), C4S(H4S), C5(H5), C5S(H5S), C6(H6), C6S(H6S),
 C7(H7), C11(H11), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19), C35(H35),
 C36(H36), C37(H37), C41(H41), C42(H42), C43(H43), C47(H47), C48(H48), C49(H49),
  C64(H64), C65(H65), C67(H67), C68(H68)
5.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C),
 C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              40139
_shelx_hkl_checksum              79508
_olex2_submission_special_instructions 'No special instructions were received'