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_4116347
_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   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            4
_cell_length_a                   12.0338(11)
_cell_length_b                   7.2535(10)
_cell_length_c                   15.9377(13)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    223(1)
_cell_measurement_theta_max      15.70
_cell_measurement_theta_min      12.05
_cell_volume                     1391.2(3)
_computing_cell_refinement       cad4/pc
_computing_data_collection       cad4/pc
_computing_data_reduction        'XCAD4B (Harms, 1996)'
_computing_molecular_graphics    'SHELXTL Rel. 5.05/VMS (Siemens, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(1)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.469
_diffrn_measurement_device_type  CAD-4
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4061
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         29.98
_diffrn_reflns_theta_min         2.56
_exptl_absorpt_coefficient_mu    1.449
_exptl_absorpt_correction_type   psi-scans
_exptl_crystal_colour            purple/violet
_exptl_crystal_density_diffrn    1.829
_exptl_crystal_F_000             792
_refine_diff_density_max         0.808
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         1094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.2996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                942
_reflns_number_total             1094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja983247t_7.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0465P)^2^+1.2996P] 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^)+(0.0465P)^2^+1.2996P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4116347