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_4119356
_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
;
C390 H310 N60 Ni10, Cl, 19(Cl O4), 4(C2 H3 N), 8(C4 H10 O)
;
_chemical_formula_sum            'C430 H422 Cl20 N64 Ni10 O84'
_chemical_formula_weight         9126.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_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                 97.353(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.568(8)
_cell_length_b                   30.857(11)
_cell_length_c                   34.260(12)
_cell_measurement_reflns_used    14245
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      59.5
_cell_measurement_theta_min      12.2
_cell_volume                     22613(14)
_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  'SHELXH-97 (Sheldrick, 1997)'
_computing_structure_solution    'SUPERFLIP (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device
;
AFC11 (Right): Eulerian 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn944+ (2x2 bin mode) CCD
;
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Confocal Mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_sigmaI/netI    0.0891
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            178848
_diffrn_reflns_theta_full        59.86
_diffrn_reflns_theta_max         59.86
_diffrn_reflns_theta_min         1.43
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.193
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.437
_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    1.340
_exptl_crystal_description       Plate
_exptl_crystal_F_000             9484
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
included as diethyl ether solvent
;
_refine_diff_density_max         0.812
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.957
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1868
_refine_ls_number_reflns         32315
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.2399
_refine_ls_R_factor_gt           0.1497
_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^)+(0.1500P)^2^+50.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3666
_refine_ls_wR_factor_ref         0.4101
_reflns_number_gt                11938
_reflns_number_total             32315
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja311285b_si_001_07.cif
_cod_data_source_block           NiClO4barreltoludine
_cod_original_cell_volume        22614(14)
_cod_database_code               4119356