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_7044070
_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         'C26 H36 Cl N10 O2 Pd'
_chemical_formula_sum            'C26 H36 Cl N10 O2 Pd'
_chemical_formula_weight         662.50
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-09-26
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2017-07-19 deposited with the CCDC.
2017-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.3960(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4316(5)
_cell_length_b                   8.8810(2)
_cell_length_c                   18.9892(5)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.828
_cell_measurement_theta_min      2.557
_cell_volume                     2949.52(13)
_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, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27638
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.828
_diffrn_reflns_theta_min         1.861
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.762
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/3 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0410 before and 0.0373 after correction.
The Ratio of minimum to maximum transmission is 0.9425.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_description       prism
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0251P)^2^+2.2423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6285
_reflns_number_total             7644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02646c2.cif
_cod_data_source_block           rh132
_cod_database_code               7044070
_shelxl_version_number           2014/6
_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. Rigid body (RIGU) restrains
 C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H19A)=Sof(C20)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C21)=Sof(H21D)=Sof(H21E)=
 Sof(H21F)=1-FVAR(1)
 Sof(H19)=Sof(C20')=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C21')=Sof(H21A)=
 Sof(H21B)=Sof(H21C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C16(H16), C19(H19), C19(H19A)
4.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C23(H23), C24(H24), C25(H25), C26(H26)
4.c 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(H20D,H20E,H20F), C20'(H20A,H20B,H20C),
 C21(H21D,H21E,H21F), C21'(H21A,H21B,H21C)
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_shelx_res_checksum              82198
_olex2_submission_special_instructions 'No special instructions were received'