Reversible Photo-isomerization of cis-[Pd(L-κS,O)2] (HL = N N-diethyl-N’-1-naphthoylthiourea) to trans-[Pd(L-κS,O)2] and the Unprecedented Formation of trans-[Pd(L-κS,N)2] in Solution.
Nkabyo, Henry A.; Procacci, Barbara; Duckett, Simon B.; Koch, Klaus R.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03672E

data_7701848
_publ_section_title
;
 Reversible Photo-isomerization of cis-[Pd(L-\kS,O)2] (HL = N
 N-diethyl-N&#x2019;-1-naphthoylthiourea) to trans-[Pd(L-\kS,O)2] and the
 Unprecedented Formation of trans-[Pd(L-\kS,N)2] in Solution.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03672E
_journal_year                    2019
_chemical_formula_moiety         'C32 H34 N4 O2 Pd S2'
_chemical_formula_sum            'C32 H34 N4 O2 Pd S2'
_chemical_formula_weight         677.15
_chemical_melting_point          158.0(10)
_chemical_name_systematic
cis-bis(N,N-diethyl-N?-1-naphthoylthioureato-S,O)palladium(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-10-22 deposited with the CCDC.	2019-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.067(8)
_cell_length_b                   9.3233(18)
_cell_length_c                   15.204(3)
_cell_measurement_reflns_used    2972
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.32
_cell_measurement_theta_min      2.23
_cell_volume                     6105(2)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_molecular_graphics
'X-Seed (Barbour, 2001; Atwood & Barbour, 2003)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2016)'
_diffrn_ambient_pressure         101.3
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       54
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34331
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.286
_diffrn_reflns_theta_min         1.891
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker SMART APEX'
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'symmetry-related measurement'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_meas      1.473
_exptl_crystal_density_method    not-measured
_exptl_crystal_description       rod
_exptl_crystal_F_000             2784
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.208
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.884
_exptl_transmission_factor_min   0.821
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.708
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0381P)^2^+2.3574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1044
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4936
_reflns_number_total             7077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03672e2.cif
_cod_data_source_block           C
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '157-159' was changed to
'158.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7701848
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.788
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              86518