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_4343495
_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         'C69 H79 N3 O2 Pd'
_chemical_formula_sum            'C69 H79 N3 O2 Pd'
_chemical_formula_weight         1088.80
_chemical_name_systematic        Pd(m-C(O)H-C6H4NO)(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_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                 99.0140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.6611(10)
_cell_length_b                   11.7309(4)
_cell_length_c                   20.0171(8)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.406
_cell_measurement_theta_min      2.326
_cell_volume                     5951.3(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
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0325
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            46710
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.406
_diffrn_reflns_theta_min         1.607
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0820 before and 0.0393 after correction.
The Ratio of minimum to maximum transmission is 0.9253.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.658
_refine_diff_density_min         -0.679
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         12219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+8.5174P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10660
_reflns_number_total             12219
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01252_si_002.cif
_cod_data_source_block           jfig866
_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               4343495
_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(C66A) = Uanis(C66)
Uanis(C64A) = Uanis(C68)
Uanis(C63A) = Uanis(C63)
Uanis(O2A) = Uanis(O2)
Uanis(C69) = Uanis(C69A)
3. Others
 Sof(C68A)=Sof(H68A)=Sof(C67A)=Sof(H67A)=Sof(C66A)=Sof(H66A)=Sof(C65A)=
 Sof(C69A)=Sof(H69A)=Sof(O2A)=Sof(C64A)=Sof(H64A)=Sof(C63A)=1-FVAR(1)
 Sof(C63)=Sof(C68)=Sof(H68)=Sof(C67)=Sof(H67)=Sof(C66)=Sof(H66)=Sof(C65)=
 Sof(C69)=Sof(H69)=Sof(C64)=Sof(H64)=Sof(O2)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C27(H27), C15(H15), C60(H60), C57(H57), C48(H48), C45(H45), C30(H30), C18(H18)
4.b Aromatic/amide H refined with riding coordinates:
 C68(H68), C67(H67), C66(H66), C69(H69), C64(H64), C55(H55), C54(H54),
 C53(H53), C37(H37), C36(H36), C35(H35), C43(H43), C42(H42), C41(H41), C7(H7),
 C6(H6), C5(H5), C23(H23), C24(H24), C25(H25), C11(H11), C12(H12), C13(H13),
 C68A(H68A), C67A(H67A), C66A(H66A), C69A(H69A), C64A(H64A)
4.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C61(H61A,H61B,H61C), C58(H58A,H58B,H58C), C59(H59A,H59B,
 H59C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C47(H47A,H47B,H47C), C46(H46A,
 H46B,H46C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C),
 C32(H32A,H32B,H32C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              6353
_shelx_hkl_checksum              83894
_olex2_submission_special_instructions 'No special instructions were received'