Further Study of the Linear Trinickel(II) Complex of Dipyridylamide
Rodolphe Clérac; F. Albert Cotton; Kim R. Dunbar; Carlos A. Murillo; Isabel Pascual; Xiaoping Wang; Inorganic Chemistry 38 (1999) 2655–2657; doi:10.1021/ic990006t

data_4322047
_publ_contact_author_address
; Dept. of Chemistry
  P.O. Box 30012
  Texas A&M University
  College Station, TX 77842-3012
  USA
;
_publ_contact_author_email       cotton@tamu.edu
_publ_contact_author_fax         '(409) 845 9351'
_publ_contact_author_name        'F.A. Cotton'
_publ_contact_author_phone       '(409) 845 4432'
_publ_section_title
;
 Further Study of the Linear Trinickel(II) Complex of Dipyridylamide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2655
_journal_page_last               2657
_journal_paper_doi               10.1021/ic990006t
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesis
_chemical_formula_structural     Ni3(dpa)4Cl2.2CH2Cl2
_chemical_formula_sum            'C42 H36 Cl6 N12 Ni3'
_chemical_formula_weight         1097.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_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            8
_cell_length_a                   27.3046(7)
_cell_length_b                   27.3046(7)
_cell_length_c                   12.2452(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.9
_cell_measurement_theta_min      9.05
_cell_volume                     9129.3(4)
_computing_cell_refinement       'MADNES (Pflugrath & Messerschmidt, 1992)'
_computing_data_collection       'MADNES (Pflugrath & Messerschmidt, 1992)'
_computing_data_reduction        'SHELXTL (Sheldrick, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1996)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1996)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            19140
_diffrn_reflns_theta_max         22.45
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         'None (area detector data)'
_exptl_absorpt_coefficient_mu    1.623
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             4464
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         5930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_obs          0.0392
_refine_ls_shift/esd_max         -0.007
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+57.8378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0996
_refine_ls_wR_factor_obs         0.0978
_reflns_number_observed          5743
_reflns_number_total             5931
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990006t_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+57.8378P] 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^)+(0.0400P)^2^+57.8378P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322047