Pd-complex driven formation of single-chain nanoparticles
Willenbacher, Johannes; Altintas, Ozcan; Trouillet, Vanessa; Knöfel, Nicolai; Monteiro, Michael J.; Roesky, Peter W.; Barner-Kowollik, Christopher; Polym. Chem. 6 (2015) 4358–; doi:10.1039/C5PY00389J

data_1519455
_publ_section_title
;
 Pd-complex driven formation of single-chain nanoparticles
;
_journal_issue                   24
_journal_name_full               'Polym. Chem.'
_journal_page_first              4358
_journal_paper_doi               10.1039/C5PY00389J
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C56 H50 Cl2 O4 P2 Pd'
_chemical_formula_sum            'C56 H50 Cl2 O4 P2 Pd'
_chemical_formula_weight         1026.20
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-04-17 deposited with the CCDC.
2015-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                89.46(3)
_cell_angle_beta                 87.53(3)
_cell_angle_gamma                73.09(3)
_cell_formula_units_Z            2
_cell_length_a                   10.118(2)
_cell_length_b                   14.622(3)
_cell_length_c                   17.316(4)
_cell_measurement_reflns_used    15145
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      1.87
_cell_volume                     2448.8(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2013)'
_computing_structure_solution    'ShelXS (Sheldrick, 2013)'
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0607
_diffrn_reflns_av_unetI/netI     0.0804
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            18856
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.869
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.600
_exptl_absorpt_correction_T_max  0.9600
_exptl_absorpt_correction_T_min  0.8876
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.095
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.866
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         9493
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.866
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0320P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6557
_reflns_number_total             9493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5py00389j2.cif
_cod_data_source_block           nk11(2)
_cod_depositor_comments
'Adding full bibliography for 1519454--1519455.cif.'
_cod_original_cell_volume        2448.8(9)
_cod_database_code               1519455
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C27A(0.5) H27A(0.5) H27B(0.5) C28B(0.5) H28D(0.5) H28E(0.5)
 H28F(0.5) C27B(0.5) H27C(0.5) H27D(0.5) C28A(0.5) H28A(0.5) H28B(0.5) H28C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C48(H48A,H48B), C55(H55A,H55B), C27A(H27A,H27B), C27B(H27C,
 H27D)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C22(H22), C23(H23), C25(H25),
  C26(H26), C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36),
 C37(H37), C38(H38), C39(H39), C40(H40), C42(H42), C43(H43), C45(H45), C46(H46),
  C50(H50), C51(H51), C53(H53), C54(H54)
3.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C28B(H28D,H28E,H28F), C28A(H28A,H28B,H28C)
;
_shelx_res_checksum              84330
_olex2_submission_special_instructions 'No special instructions were received'