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_4343500
_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         'C111 H126 N6 O3 Pd3'
_chemical_formula_sum            'C111 H126 N6 O3 Pd3'
_chemical_formula_weight         1911.37
_chemical_name_common            '[Pd(PhNO)(CNArDipp2)]3'
_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   mixed
_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                 97.594(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.368(3)
_cell_length_b                   18.616(3)
_cell_length_c                   30.754(6)
_cell_measurement_reflns_used    9792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      2.78
_cell_volume                     9856(3)
_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 0.972
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Ultra'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_laue_measured_fraction_full 0.972
_diffrn_reflns_laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            55232
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        68.000
_diffrn_reflns_theta_max         70.808
_diffrn_reflns_theta_min         2.781
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.773
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.535
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'red orange'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             3984
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1312
_refine_ls_number_reflns         17729
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0850
_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^)+(0.0831P)^2^+32.7551P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2133
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15691
_reflns_number_total             17729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b01252_si_002.cif
_cod_data_source_block           jfigcu25
_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.

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               4343500
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.647
_shelx_estimated_absorpt_t_min   0.535
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-H17A
 0.95 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C73A) \\sim Ueq, Uanis(C73B) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C73A) = Uanis(C73B)
Uanis(N1) = Uanis(N1B)
4. Others
 Sof(Pd3B)=Sof(Pd1B)=Sof(Pd2B)=Sof(H24A)=Sof(H12A)=Sof(H11A)=Sof(H23A)=
 Sof(H18A)=Sof(H17A)=Sof(N1B)=Sof(N2B)=Sof(C7B)=Sof(C8B)=Sof(H8B)=Sof(C14B)=
 Sof(H14B)=Sof(C13B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10S)=Sof(C15B)=Sof(H15B)=
 Sof(C16B)=Sof(H16B)=Sof(N3B)=Sof(C20B)=Sof(H20B)=Sof(C19B)=Sof(C21B)=Sof(H21B)=
 Sof(C22B)=Sof(H22B)=1-FVAR(1)
 Sof(Pd1)=Sof(Pd2)=Sof(Pd3)=Sof(H24)=Sof(H12)=Sof(H11)=Sof(H23)=Sof(C20)=
 Sof(H20)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(H9)=Sof(C7)=Sof(C8)=Sof(H8)=Sof(N1)=
 Sof(N2)=Sof(N3)=Sof(H18)=Sof(C19)=Sof(C13)=Sof(C14)=Sof(H14)=Sof(C22)=Sof(H22)=
 Sof(C21)=Sof(H21)=Sof(H17)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1)
 Sof(C73A)=Sof(H73A)=Sof(H73B)=Sof(H73C)=1-FVAR(2)
 Sof(C73B)=Sof(H73D)=Sof(H73E)=Sof(H73F)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C100(H100), C45(H45), C80(H80), C77(H77), C103(H103), C42(H42), C74(H74),
 C71(H71), C51(H51), C109(H109), C48(H48), C106(H106)
5.b Aromatic/amide H refined with riding coordinates:
 C86(H86), C98(H98), C57(H57), C63(H63), C28(H28), C62(H62), C67(H67),
 C33(H33), C24(H24), C12(H12), C97(H97), C32(H32), C11(H11), C26(H26), C34(H34),
  C23(H23), C40(H40), C38(H38), C20(H20), C85(H85), C55(H55), C96(H96),
 C84(H84), C39(H39), C91(H91), C56(H56), C27(H27), C92(H92), C10(H10), C61(H61),
  C68(H68), C69(H69), C9(H9), C8(H8), C18(H18), C14(H14), C22(H22), C21(H21),
 C17(H17), C15(H15), C16(H16), C90(H90), C8B(H8B), C14B(H14B), C9B(H9B),
 C10B(H10S), C15B(H15B), C16B(H16B), C20B(H20B), C21B(H21B), C22B(H22B)
5.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C46(H46A,H46B,
 H46C), C101(H10A,H10B,H10C), C50(H50A,H50B,H50C), C105(H10D,H10E,H10F),
 C78(H78A,H78B,H78C), C52(H52A,H52B,H52C), C104(H10G,H10H,H10I), C49(H49A,H49B,
 H49C), C81(H81A,H81B,H81C), C43(H43A,H43B,H43C), C102(H10J,H10K,H10L),
 C72(H72A,H72B,H72C), C108(H10M,H10N,H10O), C111(H11B,H11C,H11D), C107(H10P,
 H10Q,H10R), C110(H11E,H11F,H11G), C79(H79A,H79B,H79C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C82(H82A,H82B,H82C), C73A(H73A,H73B,H73C), C73B(H73D,H73E,
 H73F)
;
_shelx_res_checksum              8095
_shelx_hkl_checksum              27967
_olex2_submission_special_instructions 'No special instructions were received'