Pinwheel motifs: formation of unusual homo- and hetero-nuclear aggregates via bridging thiolates
Amoroso, Angelo J.; Chung, Simon S. M.; Spencer, Douglas J. E.; Danks, Jonathan P.; Glenny, Mark W.; Blake, Alexander J.; Cooke, Paul A.; Wilson, Claire; Schröder, Martin; Chemical Communications (Cambridge, United Kingdom)  (2003) 2020–2021; doi:10.1039/b303851c

data_7103829
_publ_section_title
;
 Pinwheel motifs: formation of unusual homo- and hetero-nuclear
 aggregates via bridging thiolates
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   16
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2020
_journal_page_last               2021
_journal_paper_doi               10.1039/b303851c
_journal_year                    2003
_chemical_formula_sum            'C44 H92 B4 F16 N12 Pd6 S8'
_chemical_formula_weight         2031.42
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   'geometrically placed, MeCN from delta-F'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.182(7)
_cell_angle_beta                 89.969(8)
_cell_angle_gamma                76.473(7)
_cell_formula_units_Z            2
_cell_length_a                   11.594(5)
_cell_length_b                   13.393(6)
_cell_length_c                   25.598(11)
_cell_measurement_reflns_used    2726
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2
_cell_volume                     3763(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.091
_diffrn_reflns_av_sigmaI/netI    0.190
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            24288
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.61
_exptl_absorpt_coefficient_mu    1.704
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1999)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             2016
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.39
_refine_diff_density_min         -1.46
_refine_diff_density_rms         0.27
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.98
_refine_ls_hydrogen_treatment    'Riding model MeCN as rigid rotor'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         13033
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      0.97
_refine_ls_R_factor_all          0.179
_refine_ls_R_factor_gt           0.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.155P)^2^P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.245
_refine_ls_wR_factor_ref         0.288
_reflns_number_gt                6448
_reflns_number_total             16451
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303851c.txt
_cod_data_source_block           PDN2S2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7103829