Polynuclear Nickel(II) Complexes: A Magnetostructural Study of NiII4, NiII6, and NiII9 Species with Oxime Ligands
Biplab Biswas; Ulrich Pieper; Thomas Weyhermüller; Phalguni Chaudhuri; Inorganic Chemistry 48 (2009) 6781–6793; doi:10.1021/ic9007608

data_4302745
_publ_section_title
;
Polynuclear Nickel(II) Complexes: A Magnetostructural Study of NiII4,
NiII6, and NiII9 Species with Oxime Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6781
_journal_page_last               6793
_journal_paper_doi               10.1021/ic9007608
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'C50 H80 N30 Ni9 O22, 4(Cl O4), 8(C2 H3 N), H2 O'
_chemical_formula_sum            'C66 H106 Cl4 N38 Ni9 O39'
_chemical_formula_weight         2726.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.789(3)
_cell_angle_beta                 91.733(3)
_cell_angle_gamma                110.043(3)
_cell_formula_units_Z            2
_cell_length_a                   16.7841(6)
_cell_length_b                   16.9192(6)
_cell_length_c                   23.7893(9)
_cell_measurement_temperature    100(2)
_cell_volume                     6012.8(4)
_computing_cell_refinement       'Nonius Collect Software'
_computing_data_collection       'Nonius Collect Software'
_computing_data_reduction        'Nonius Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
'1193 images at 0.8 deg. stepwise rotation in omega and phi, 72 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            137520
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    1.553
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_correction_T_min  0.8022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Vers. 2006/1, Bruker AXS (2006)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent parallelepiped'
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.984
_refine_diff_density_min         -1.447
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1515
_refine_ls_number_reflns         43102
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0440
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0699P)^2^+6.0866P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1253
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                33607
_reflns_number_total             43102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9007608_si_002_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_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_database_code               4302745