Synthesis and redox chemistry of Pd(ii) complexes of a pincer verdazyl ligand.
Sanz, Corey A.; Patrick, Brian O.; Hicks, Robin G.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 12674–12683; doi:10.1039/c9dt02549a

data_7700743
_publ_section_title
;
 Synthesis and redox chemistry of Pd(ii) complexes of a pincer verdazyl
 ligand.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12674
_journal_page_last               12683
_journal_paper_doi               10.1039/c9dt02549a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C17 H18 N7 O Pd, 2(B F4)'
_chemical_formula_sum            'C17 H18 B2 F8 N7 O Pd'
_chemical_formula_weight         616.40
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                81.951(2)
_cell_angle_beta                 83.335(2)
_cell_angle_gamma                85.737(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9377(11)
_cell_length_b                   11.1851(16)
_cell_length_c                   12.3025(18)
_cell_measurement_reflns_used    9558
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.59
_cell_volume                     1072.3(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 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0346
_diffrn_reflns_av_unetI/netI     0.0349
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17152
_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         27.978
_diffrn_reflns_theta_min         1.681
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.963
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.885
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0473 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.9020.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_description       irregular
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.983
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0421P)^2^+2.9400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4449
_reflns_number_total             5165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02549a2.cif
_cod_data_source_block           rh148
_cod_depositor_comments
'Adding full bibliography for 7700743--7700746.cif.'
_cod_database_code               7700743
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.861
_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.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              29273
_olex2_submission_special_instructions 'No special instructions were received'