Synthesis and redox reactions of bis(verdazyl) palladium complexes
Sanz, Corey A.; McKay, Zach R.; Patrick, Brian O.; MacLean, Shaun W.C.; Hicks, Robin G.; Dalton Trans.  (2017) –; doi:10.1039/C7DT02646C

data_7044071
_publ_section_title
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 Synthesis and redox reactions of bis(verdazyl) palladium complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02646C
_journal_year                    2017
_chemical_formula_moiety         'C28 H42 N10 O3 Pd S, 2(B F4)'
_chemical_formula_sum            'C28 H42 B2 F8 N10 O3 Pd S'
_chemical_formula_weight         878.79
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.149(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2988(4)
_cell_length_b                   22.7666(9)
_cell_length_c                   18.2185(7)
_cell_measurement_reflns_used    8378
_cell_measurement_temperature    90
_cell_measurement_theta_max      56.950
_cell_measurement_theta_min      3.107
_cell_volume                     3854.2(3)
_computing_cell_refinement       'SAINT v8.34A (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, 2015)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.737
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.737
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17665
_diffrn_reflns_point_group_measured_fraction_full 0.737
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         56.968
_diffrn_reflns_theta_min         3.108
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.129
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.472
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1129 before and 0.0653 after correction.
The Ratio of minimum to maximum transmission is 0.5799.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       needle
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.276
_refine_diff_density_min         -1.518
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0765
_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^)+(0.0211P)^2^+57.4903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1904
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3919
_reflns_number_total             5136
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02646c2.cif
_cod_data_source_block           rh149
_cod_database_code               7044071
_shelxl_version_number           2014/6
_olex2_refinement_description
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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(O3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.2
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(B2)=Sof(F10)=Sof(F11)=Sof(F13)=Sof(F16)=1-FVAR(1)
 Sof(B3)=Sof(F9)=Sof(F12)=Sof(F14)=Sof(F15)=FVAR(1)
 Sof(F1)=Sof(F4)=Sof(F6)=Sof(F8)=1-FVAR(2)
 Sof(F2)=Sof(F3)=Sof(F5)=Sof(F7)=FVAR(2)
5.a Free rotating group:
 S1(C27,C28,H27A,H27B,H27C,O3), B2(F10,F11,F13,F16), B3(F9,F12,F14,F15)
5.b Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C16(H16), C19(H19)
5.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24), C25(H25), C26(H26)
5.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C17(H17A,
 H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C),
 C28(H28A,H28B,H28C)
;
_shelx_res_checksum              17783
_olex2_submission_special_instructions 'No special instructions were received'