Five Discrete Multinuclear Metal-Organic Assemblies from One Ligand: Deciphering the Effects of Different Templates
Imogen A. Riddell; Yana R. Hristova; Jack K. Clegg; Christopher S. Wood; Boris Breiner; Jonathan R. Nitschke; Journal of the American Chemical Society 135 (2013) 2723–2733; doi:10.1021/ja311285b

data_4119355
_publ_section_title
;
 Five Discrete Multinuclear Metal-Organic Assemblies from One Ligand:
 Deciphering the Effects of Different Templates
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2723
_journal_page_last               2733
_journal_paper_doi               10.1021/ja311285b
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety
;
C208 H156 N32 Ni6, 6(C6 H14 O), 8(C2 H3 N), 12(C O3 F3 S)
;
_chemical_formula_sum            'C272 H284 F36 N40 Ni6 O42 S12'
_chemical_formula_weight         6206.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           181
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      181
_symmetry_space_group_name_Hall  'P 64 2 (0 0 2)'
_symmetry_space_group_name_H-M   'P 64 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   21.9120(2)
_cell_length_b                   21.9120(2)
_cell_length_c                   54.0560(9)
_cell_measurement_reflns_used    411853
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     22477.0(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics
;ORTEP-3 (Farrugia, 1997)
WINGX-32 (Farrugia, 1999) 
;
_computing_publication_material  'enCIFer 1.1 (CCDC, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type
;
Bruker-Nonius Roper CCD camera on \k-goniostat
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0726
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            106823
_diffrn_reflns_theta_full        20.82
_diffrn_reflns_theta_max         20.82
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.777258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       rhombus
_exptl_crystal_F_000             9648
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
included as residual solvent and missing anions
;
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.16(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7821
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.1208
_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^)+(0.1862P)^2^+74.6980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3155
_refine_ls_wR_factor_ref         0.3205
_reflns_number_gt                7262
_reflns_number_total             7821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311285b_si_001_06.cif
_cod_data_source_block           NiGrid
_cod_original_sg_symbol_Hall
;
P 64 2c (00-1)
;
_cod_database_code               4119355