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_4119354
_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
;
C156 H132 N24 Ni4 , 6.25(C2 H3 N), 6(C4 H10 O), 8(C F S3 O3)
;
_chemical_formula_sum            'C200.5 H210.75 F24 N30.25 Ni4 O30 S8'
_chemical_formula_weight         4471.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_Int_Tables_number      190
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_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            4
_cell_length_a                   24.581(5)
_cell_length_b                   24.581(5)
_cell_length_c                   41.330(11)
_cell_measurement_reflns_used    36508
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.6
_cell_measurement_theta_min      0.9
_cell_volume                     21627(8)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)
;
_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      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
'Rigaku Saturn 724+ detector on Crystal Logic diffractometer'
_diffrn_measurement_method       '\w  scans'
_diffrn_radiation_monochromator  'silicon double crystal'
_diffrn_radiation_source         'Diamond beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0519
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            128263
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.719
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrystalClear-SM Expert 2.0 r5 (Rigaku, 2010)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       shard
_exptl_crystal_F_000             9286
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.005
_exptl_crystal_size_min          0.005
_platon_squeeze_details
;
included as diethyl ether molecules
;
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     764
_refine_ls_number_reflns         10497
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0989
_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^)+(0.1843P)^2^+26.7611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2713
_refine_ls_wR_factor_ref         0.2740
_reflns_number_gt                10147
_reflns_number_total             10497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311285b_si_001_05.cif
_cod_data_source_block           NiOTf
_cod_original_cell_volume        21628(8)
_cod_original_formula_sum        'C200.50 H210.75 F24 N30.25 Ni4 O30 S8'
_cod_database_code               4119354