Tunable Molecular Distortion in a Nickel Complex Coupled to a Reversible Phase Transition in the Crystalline State
Larry R. Falvello; Michael A. Hitchman; Fernando Palacio; Isabel Pascual; Arthur J. Schultz; Horst Stratemeier; Milagros Tomás; Esteban P. Urriolabeitia; Dianna M. Young; Journal of the American Chemical Society 121 (1999) 2808–2819; doi:10.1021/ja983247t

data_4116342
_publ_section_title
;
 Tunable Molecular Distortion in a Nickel Complex Coupled to a Reversible
 Phase Transition in the Crystalline State
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2808
_journal_page_last               2819
_journal_paper_doi               10.1021/ja983247t
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C6 H16 N10 Ni O6'
_chemical_formula_weight         383.00
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.014(2)
_cell_length_b                   7.219(2)
_cell_length_c                   15.805(2)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      15.8
_cell_measurement_theta_min      12.1
_cell_volume                     1370.8(5)
_computing_cell_refinement       CAD4/PC
_computing_data_collection       CAD4/PC
_computing_data_reduction        xcad4b
_computing_molecular_graphics    XPW
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            666
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.58
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.856
_exptl_crystal_description       'regular block'
_exptl_crystal_F_000             792
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.360
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.096
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_hydrogen_treatment    free
_refine_ls_matrix_type           full
_refine_ls_number_parameters     80
_refine_ls_number_reflns         613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_obs          0.0371
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.9982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0994
_refine_ls_wR_factor_obs         0.0917
_reflns_number_observed          565
_reflns_number_total             666
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja983247t_2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.9982P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+0.9982P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1370.7(5)
_cod_database_code               4116342