One pot-synthesis of chiral Ni6 clusters involving Ni3 subunits: a combined structural, magnetic and DFT study.
Fondo, Matilde; Ocampo, Noelia; García-Deibe, Ana M; Cano, Joan; Sanmartín, Jesús; Dalton transactions (Cambridge, England : 2003) 39 (2010) 10888–10899; doi:10.1039/c0dt00659a

data_7026747
_publ_section_title
;
 One pot-synthesis of chiral Ni6 clusters involving Ni3 subunits: a
 combined structural, magnetic and DFT study.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10888
_journal_page_last               10899
_journal_paper_doi               10.1039/c0dt00659a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety
'C60 H69 N11 Ni6 O16, 2(C H4 O), 2(C2 H3 N), H2 O'
_chemical_formula_sum            'C66 H85 N13 Ni6 O19'
_chemical_formula_weight         1716.73
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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
_cell_angle_beta                 90.772(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.765(3)
_cell_length_b                   12.792(3)
_cell_length_c                   21.443(5)
_cell_measurement_reflns_used    951
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.375
_cell_measurement_theta_min      2.225
_cell_volume                     3501.1(14)
_computing_cell_refinement       'BRUKER Smart'
_computing_data_collection       'BRUKER Smart'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-2004 (Burla, 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker CCD SMART1000 '
_diffrn_measurement_method       'omega and phi scans'
_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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            29609
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        0.15
_exptl_absorpt_coefficient_mu    1.663
_exptl_absorpt_correction_T_max  0.9518
_exptl_absorpt_correction_T_min  0.5087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.007(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         12876
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0257P)^2^+3.8586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                10744
_reflns_number_total             12876
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00659a.txt
_cod_data_source_block           3_H2O_2MeOH_2MeCN
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3501.0(13)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7026747