Consecutive modular ligation as an access route to palladium containing polymers
Lang, Christiane; Pahnke, Kai; Kiefer, Claude; Goldmann, Anja S.; Roesky, Peter W.; Barner-Kowollik, Christopher; Polymer Chemistry 4 (2013) 5456–; doi:10.1039/c3py00648d

data_1514893
_publ_section_title
;
 Consecutive modular ligation as an access route to palladium containing
 polymers
;
_journal_issue                   21
_journal_name_full               'Polymer Chemistry'
_journal_page_first              5456
_journal_paper_doi               10.1039/c3py00648d
_journal_volume                  4
_journal_year                    2013
_chemical_formula_moiety
'C23 H19 Cl N7 Pd, C2 H6 Cl3 O Pd S, 2(C2 H6 O S)'
_chemical_formula_sum            'C29 H37 Cl4 N7 O3 Pd2 S3'
_chemical_formula_weight         982.43
_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
_audit_creation_date             2013-05-15
_audit_creation_method
;
   Olex2 1.2
   (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                109.67(3)
_cell_angle_beta                 102.90(3)
_cell_angle_gamma                95.46(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6458(17)
_cell_length_b                   13.837(3)
_cell_length_c                   17.394(4)
_cell_measurement_reflns_used    11365
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.14
_cell_measurement_theta_min      1.59
_cell_volume                     1876.8(9)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H.
Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1020
_diffrn_reflns_av_unetI/netI     0.1040
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12065
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.251
_diffrn_reflns_theta_min         1.591
_exptl_absorpt_coefficient_mu    1.451
_exptl_absorpt_correction_T_max  0.9506
_exptl_absorpt_correction_T_min  0.7627
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.738
_exptl_crystal_description       needle
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.041
_refine_diff_density_max         2.679
_refine_diff_density_min         -1.951
_refine_diff_density_rms         0.237
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6552
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0797
_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^)+(0.1347P)^2^]
  where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1915
_refine_ls_wR_factor_ref         0.2102
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4222
_reflns_number_total             6552
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3py00648d.txt
_cod_data_source_block           4
_cod_original_cell_volume        1876.9(8)
_cod_database_code               1514893
_olex2_refinement_description
;
1. Fixed Uiso
  At 1.2 times of:
   All C(H) groups
  At 1.5 times of:
   All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(S3B) = Uanis(O3B) = Uanis(C28B) = Uanis(C29B)
3. Same fragment restrains
{S2, O2, C26, C27}
as
{S3A, O3A, C28A, C29A}
{S2, O2, C26, C27}
as
{S3B, O3B, C28B, C29B}
4. Others
  Fixed Sof: S3A(0.75) O3A(0.75) C28A(0.75) H28A(0.75) H28B(0.75) H28C(0.75)
  C29A(0.75) H29A(0.75) H29B(0.75) H29C(0.75) S3B(0.25) O3B(0.25) C28B(0.25)
  H28D(0.25) H28E(0.25) H28F(0.25) C29B(0.25) H29D(0.25) H29E(0.25)
H29F(0.25)
5.a Aromatic/amide H refined with riding coordinates:
  C1(H1), C2(H2), C5(H5), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13),
  C16(H16), C18(H18), C19(H19), C21(H21), C22(H22)
5.b Idealised Me refined as rotating group:
  C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C12(H12A,H12B,H12C),
C23(H23A,H23B,
  H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C28A(H28A,H28B,H28C),
  C29A(H29A,H29B,H29C), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F)
;
_shelx_hkl_checksum              6140