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_7103830
_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            'C17 H34 Cu2 F12 Ni3 P2 S12'
_chemical_formula_weight         1216.32
_chemical_name_common
;Tris-Nickel 3,7-dithianonane-1,9-dithiolate bis-copper
hexaflurophosphate
;
_chemical_name_systematic
;
Tris-Nickel 3,7-dithianonane-1,9-dithiolate bis-copper
hexaflurophosphate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   'geometrically located'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   'difference Fourier syntheses'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.466(3)
_cell_length_b                   22.546(7)
_cell_length_c                   12.156(7)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      16.5
_cell_measurement_theta_min      10.5
_cell_volume                     4787(3)
_computing_cell_refinement       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996a)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996b)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Stoe Stadi-4 four-circle'
_diffrn_measurement_method       omega-theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0828
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4591
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.73
_diffrn_standards_decay_%        '+/- 6.5% linear increase'
_diffrn_standards_interval_time  '60 min'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.683
_exptl_absorpt_correction_T_max  0.565
_exptl_absorpt_correction_T_min  0.499
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED (Stoe & Cie, 1997b)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.54
_refine_diff_density_min         -0.94
_refine_diff_density_rms         0.23
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.20
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4324
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.18
_refine_ls_R_factor_all          0.187
_refine_ls_R_factor_gt           0.127
_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^)+(0.1025P)^2^+179.22P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.296
_refine_ls_wR_factor_ref         0.354
_reflns_number_gt                2788
_reflns_number_total             4324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303851c.txt
_cod_data_source_block           nicus8
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7103830