Mapping the influence of ligand electronics on the spectroscopic and <sup>1</sup>O<sub>2</sub> sensitization characteristics of Pd(II) biladiene complexes bearing phenyl-alkynyl groups at the 2- and 18-positions.
Martin, Maxwell I.; Pham, Trong-Nhan; Ward, Kaytlin N.; Rice, Anthony T.; Hertler, Phoebe R.; Yap, Glenn P. A.; Gilmartin, Philip H.; Rosenthal, Joel; Dalton transactions (Cambridge, England : 2003)  (2023) –; doi:10.1039/d3dt00691c

data_7713086
_publ_section_title
;
 Mapping the influence of ligand electronics on the spectroscopic and
 <sup>1</sup>O<sub>2</sub> sensitization characteristics of Pd(II)
 biladiene complexes bearing phenyl-alkynyl groups at the 2- and
 18-positions.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d3dt00691c
_journal_year                    2023
_chemical_formula_moiety         'C51 H22 F16 N4 Pd, C7 H8, [C7 H8]'
_chemical_formula_sum            'C65 H38 F16 N4 Pd'
_chemical_formula_weight         1285.39
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28cf03
_audit_creation_date             2021-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.12.01 svn.r5f60950 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-07-13 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.264(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.6184(9)
_cell_length_b                   15.4765(7)
_cell_length_c                   34.4992(15)
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    150.0
_cell_measurement_theta_max      75.30
_cell_measurement_theta_min      3.13
_cell_volume                     11000.1(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150.0
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.948
_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  0.0668
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            155904
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.059
_diffrn_reflns_theta_min         2.454
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.617
_exptl_absorpt_correction_T_max  0.7540
_exptl_absorpt_correction_T_min  0.4847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1603 before and 0.1125 after correction.
The Ratio of minimum to maximum transmission is 0.6428.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       needle
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.309
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.038
_refine_diff_density_max         1.431
_refine_diff_density_min         -1.189
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1411
_refine_ls_number_reflns         21799
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0636
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+53.8793P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1568
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18883
_reflns_number_total             21799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00691c2.cif
_cod_data_source_block           joer322_sq
_cod_database_code               7713086
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.401
_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. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim
C27 \\sim C28: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
F14 \\sim F15 \\sim F16 \\sim C48 \\sim C51: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
Uanis(F1) = Uanis(F14)
Uanis(F2) = Uanis(F15)
Uanis(F3) = Uanis(F16)
3. Rigid body (RIGU) restrains
 F1, F2, F3, C22, C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F14, F15, F16, C48, C51
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C19(H19),
 C23(H23), C24(H24), C26(H26), C27(H27), C46(H46), C47(H47), C49(H49), C50(H50),
  C1(H1), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C19(H19),
 C23(H23), C24(H24), C26(H26), C27(H27), C46(H46), C47(H47), C49(H49), C50(H50),
  C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7)
4.b Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C1(H1A,H1B,H1C), C1(H1A,H1B,H1C)
;
_shelx_res_checksum              71857
_shelx_fab_checksum              27362
_platon_squeeze_special_details
;
A solvent mask was calculated and 402 electrons were 
found in a volume of 1704\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
[+ solvents] per Asymmetric Unit 
which account for 400 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'