Rationally designed chiral Ni5L6 clusters with the in situ generated tridentate ligand. Hydrothermal synthesis, crystal structures, morphology and magnetic properties
Feng, Sisi; Zhu, Miaoli; Lu, Liping; Du, Lei; Zhang, Yunbo; Wang, Tianwei; Dalton Transactions  (2009) 6385–6395; doi:10.1039/b900709a

data_7001809
_publ_section_title
;
 Rationally designed chiral Ni5L6 clusters with the in situ generated
 tridentate ligand. Hydrothermal synthesis, crystal structures,
 morphology and magnetic properties
;
_journal_issue                   32
_journal_name_full               'Dalton Transactions'
_journal_page_first              6385
_journal_page_last               6395
_journal_paper_doi               10.1039/b900709a
_journal_year                    2009
_chemical_formula_moiety
'C96 H66 N24 Ni5 O6, Br0.70, Br0.60, Br0.45, 2.25Br'
_chemical_formula_sum            'C96 H66 Br4 N24 Ni5 O6'
_chemical_formula_weight         2264.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 105.353(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.146(4)
_cell_length_b                   26.711(9)
_cell_length_c                   29.026(9)
_cell_measurement_reflns_used    16459
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4797
_cell_measurement_theta_min      2.0760
_cell_volume                     9829(5)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_data_reduction        'CrystalClear (Rigaku/MSC Inc., 2005)'
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1999)'
_computing_publication_material
;
SHELXTL/PC

Mercury Ver. 1.3 (Bruno et al., 2002)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku RAXIS-IV Imaging Plate'
_diffrn_measurement_method       CCD_Profile_fitting
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60407
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    2.632
_exptl_absorpt_correction_T_max  0.7093
_exptl_absorpt_correction_T_min  0.6485
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(HIGASHI, T. (1995). Abscor - Empirical Absorption Correction
based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan.)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             4552
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
Structure contains solvent accessible voids of 521.4 A3/per unit cell,
i.e. some 5.3% of the total volume. Data were also corrected for
disordered electron density through use of the SQUEEZE procedure.
Attempts to refine peaks of residual electron density as solvent water
molecules were unsuccessful. Derived values (formula weight, density,
absorption coefficient) do not contain the contribution of
the disordered solvent molecule.
;
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.372
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1279
_refine_ls_number_reflns         17074
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0807
_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^)+(0.1225P)^2^+22.1431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2011
_refine_ls_wR_factor_ref         0.2379
_reflns_number_gt                11736
_reflns_number_total             17074
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b900709a.txt
_cod_data_source_block           fwbr-14
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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      P21/c
_cod_database_code               7001809