Aging and Ball-Milling as Low-Energy and Environmentally Friendly Methods for the Synthesis of Pd(II) Photosensitizers
Juribašić, Marina; Halasz, Ivan; Babić, Darko; Cinčić, Dominik; Plavec, Janez; Ćurić, Manda; Organometallics 33 (2014) 1227–; doi:10.1021/om500008v

data_4082700
_publ_section_title
;
 Aging and Ball-Milling as Low-Energy and Environmentally Friendly Methods
 for the Synthesis of Pd(II) Photosensitizers
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1227
_journal_paper_doi               10.1021/om500008v
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C49 H40 Cl2 N2 O P2 Pd2, C2 H6 O'
_chemical_formula_sum            'C51 H46 Cl2 N2 O2 P2 Pd2'
_chemical_formula_weight         1064.54
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_audit_creation_date             2013-08-29T16:01:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.340(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5886(7)
_cell_length_b                   9.2766(11)
_cell_length_c                   43.509(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4663.9(7)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.3426
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  GoniometerKM4/Xcalibur,detector:Sapphire3
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       56
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            22866
_diffrn_reflns_theta_full        29.56
_diffrn_reflns_theta_max         29.56
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
(compiled Jun 10 2008,16:49:55)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.931
_refine_diff_density_min         -0.822
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.24(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         15044
_refine_ls_number_restraints     280
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_gt           0.1035
_refine_ls_shift/su_max          0.033
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+62.8478P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2706
_reflns_number_gt                7622
_reflns_number_total             15044
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500008v_si_003.cif
_cod_data_source_block           exp_2903_man_46-ok
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4082700