Nickel pivalate complexes: structural variations and magnetic susceptibility and inelastic neutron scattering studies
Chaboussant, Gr�gory; Basler, Reto; G�del, Hans-Ulrich; Ochsenbein, Stefan; Parkin, Andrew; Parsons, Simon; Rajaraman, Gopalan; Sieber, Andreas; Smith, Andrew A.; Timco, Grigore A.; Winpenny, Richard E. P.; Dalton Transactions  (2004) 2758–2766; doi:10.1039/b406112h

data_7027864
_publ_section_title
;
 Nickel pivalate complexes: structural variations and magnetic
 susceptibility and inelastic neutron scattering studies
;
_journal_issue                   17
_journal_name_full               'Dalton Transactions'
_journal_page_first              2758
_journal_page_last               2766
_journal_paper_doi               10.1039/b406112h
_journal_year                    2004
_chemical_formula_moiety         '[Ni4(OMe)4(tBuCOO)4(MeOH)4].4.5MeOH'
_chemical_formula_sum            'C32.5 H82 Ni4 O20.5'
_chemical_formula_weight         1035.82
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.929(2)
_cell_length_b                   15.433(2)
_cell_length_c                   42.067(7)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22
_cell_measurement_theta_min      20
_cell_volume                     10341(3)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'Stoe REDU4'
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_method       Omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            12302
_diffrn_reflns_theta_full        70.16
_diffrn_reflns_theta_max         70.16
_diffrn_reflns_theta_min         3.48
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.627
_exptl_absorpt_correction_T_min  0.452
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Optimised numerical correction against \y scan susing XSHAPE
;
_exptl_crystal_colour            Green
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4424
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.552
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         9096
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+34.0022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1737
_reflns_number_gt                6448
_reflns_number_total             9096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b406112hsup1.cif
_cod_data_source_block           p15agt
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Integration'
changed to 'integration' 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 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'geometric' was changed to
'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C32.50 H82 Ni4 O20.50'
_cod_database_code               7027864