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_7713085
_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_absolute_configuration ad
_chemical_formula_moiety         'C51 H22 F10 N6 Pd, 1.333[CH2Cl2]'
_chemical_formula_sum            'C52.34 H24.66 Cl2.66 F10 N6 Pd'
_chemical_formula_weight         1128.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc28cdy0
_audit_creation_date             2021-07-13
_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                 122.151(2)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   44.559(2)
_cell_length_b                   11.8743(6)
_cell_length_c                   31.6316(16)
_cell_measurement_reflns_used    9797
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      21.65
_cell_measurement_theta_min      2.36
_cell_volume                     14169.9(12)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 1.000
_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_R_equivalents  0.0699
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       -58
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            180701
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.640
_diffrn_reflns_theta_min         1.316
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0627 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.9297.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_description       block
_exptl_crystal_F_000             6743
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.074
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.648
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.143(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1842
_refine_ls_number_reflns         32729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0612P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1144
_reflns_Friedel_coverage         0.992
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                24929
_reflns_number_total             32729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00691c2.cif
_cod_data_source_block           joer288
_cod_original_cell_volume        14170.1(13)
_cod_database_code               7713085
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.788
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.857(18)
 0.143(18)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Others
 Fixed X: Pd1(0.79719)
 Fixed Z: Pd1(0.90134)
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),
 C37(H37), C38(H38), C40(H40), C41(H41), C45(H45), C46(H46), C48(H48), C49(H49),
  C1(H1), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C19(H19),
 C37(H37), C38(H38), C40(H40), C41(H41), C45(H45), C46(H46), C48(H48), C49(H49),
  C1(H1), C3(H3), C7(H7), C8(H8), C12(H12), C13(H13), C17(H17), C19(H19),
 C37(H37), C38(H38), C40(H40), C41(H41), C45(H45), C46(H46), C48(H48), C49(H49)
4.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 728 electrons were 
found in a volume of 2472\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
0.667[CH2Cl2], 0.667[CH2Cl2] per Asymmetric Unit 
which account for 672 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              64478
_shelx_fab_checksum              33690
_olex2_submission_special_instructions 'No special instructions were received'