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_7700744
_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, B F4'
_chemical_formula_sum            'C17 H18 B F4 N7 O Pd'
_chemical_formula_weight         529.59
_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             2016-07-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                82.339(3)
_cell_angle_beta                 82.935(3)
_cell_angle_gamma                77.558(3)
_cell_formula_units_Z            4
_cell_length_a                   7.0857(4)
_cell_length_b                   14.7257(9)
_cell_length_c                   21.1621(13)
_cell_measurement_reflns_used    9950
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.54
_cell_volume                     2126.8(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_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_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14498
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.949
_diffrn_reflns_theta_min         2.540
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.931
_exptl_absorpt_correction_T_max  0.9634
_exptl_absorpt_correction_T_min  0.8098
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1240 before and 0.0369 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1263 before and 0.0393 after correction.
 The Ratio of minimum to maximum transmission is 0.84.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 51449 reflections, Rint = 0.0339
 (32008 with I > 3sig(I), Rint = 0.0296)
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_description       needle
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.034
_refine_diff_density_min         -0.892
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         14498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0466P)^2^+8.1160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12555
_reflns_number_total             14498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02549a2.cif
_cod_data_source_block           rh182_sq
_cod_depositor_comments
'Adding full bibliography for 7700743--7700746.cif.'
_cod_database_code               7700744
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.768
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5869(10) 0.4131(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C3(H3), C3'(H3')
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14), C15(H15),
 C7'(H7'), C8'(H8'), C9'(H9'), C10'(H10'), C12'(H12'), C13'(H13'), C14'(H14'),
 C15'(H15')
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C4'(H4'A,H4'B,H4'C),
 C5'(H5'C,H5'A,H5'B), C17'(H17D,H17E,H17F)
;
_shelx_res_checksum              99521
_shelx_fab_checksum              81395
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'