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_7001808
_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, N O3, 3(H O), 2(H2 O)'
_chemical_formula_sum            'C96 H73 N25 Ni5 O14'
_chemical_formula_weight         2094.34
_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                 106.509(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.267(4)
_cell_length_b                   26.128(7)
_cell_length_c                   29.054(7)
_cell_measurement_reflns_used    11273
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4487
_cell_measurement_theta_min      2.0895
_cell_volume                     9656(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 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0835
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            60801
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    1.033
_exptl_absorpt_correction_T_max  0.9406
_exptl_absorpt_correction_T_min  0.8358
_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    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
The crystal structure contains voids (950.6 A3/per unit cell,
i.e. some 9.84% of the unit cell volume) filled with
a disordered solvent molecule (water). Attempts to refine peaks of
residual electron density as solvent O atom (water) and NO3 anion
were unsuccessful. Derived values (formula weight, density,
absorption coefficient) do not contain the contribution of the
disordered solvent molecule.

R factors before data are squeezed:
_refine_ls_R_factor_all 0.1450
_refine_ls_R_factor_gt 0.0933
_refine_ls_wR_factor_ref 0.2694
_refine_ls_wR_factor_gt 0.2294
;
_refine_diff_density_max         0.942
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.097
_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     1292
_refine_ls_number_reflns         16705
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1463P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2695
_reflns_number_gt                10432
_reflns_number_total             16705
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b900709a.txt
_cod_data_source_block           fwno3b-s
_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      ' P 21/c'
_cod_database_code               7001808