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_4082699
_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_formula_moiety         'C86 H72 Cl2 N4 O2 P4 Pd2'
_chemical_formula_sum            'C86 H72 Cl2 N4 O2 P4 Pd2'
_chemical_formula_weight         1601.06
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             2013-06-27T14:51:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4641(9)
_cell_length_b                   20.9734(6)
_cell_length_c                   24.7791(15)
_cell_measurement_reflns_used    6458
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      76.3637
_cell_measurement_theta_min      2.7579
_cell_volume                     7517.0(7)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
        (compiled Jan  5 2010,16:28:46)
;
_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_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Oxford Xcalibur Nova'
_diffrn_measurement_method
;
        CCD detector
;
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            28024
_diffrn_reflns_theta_full        76.55
_diffrn_reflns_theta_max         76.55
_diffrn_reflns_theta_min         2.76
_exptl_absorpt_coefficient_mu    5.719
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.57481
_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            red
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.063
_refine_diff_density_min         -0.891
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.03
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     883
_refine_ls_number_reflns         14588
_refine_ls_number_restraints     305
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_gt           0.1048
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+64.5135P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2637
_reflns_number_gt                10564
_reflns_number_total             14588
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500008v_si_003.cif
_cod_data_source_block           manda-c2dmanabttp-dmf-1
_cod_database_code               4082699