Experimental charge-density study on the nickel(II) coordination complex [Ni(H~3~<i>L</i>)][NO~3~][PF~6~] [H~3~<i>L</i> = <i>N</i>,<i>N</i>',<i>N</i>''-tris(2-hydroxy-3-methylbutyl)-1,4,7-triazacyclononane]: a reappraisal
Farrugia, L. J.; Frampton, C. S.; Howard, J. A. K.; Mallinson, P. R.; Peacock, R. D.; Smith, G. T.; Stewart, B.; Acta Crystallographica Section B 62 (2006) 236–244; doi:10.1107/S0108768106000802

data_2100424
_publ_section_title
;Experimental charge-density study on the nickel(II) coordination complex
 [Ni(H~3~<i>L</i>)][NO~3~][PF~6~] [H~3~<i>L</i> =
 <i>N</i>,<i>N</i>',<i>N</i>''-tris(2-hydroxy-3-methylbutyl)-1,4,7-triazacyclononane]:
 a reappraisal
;
_journal_coeditor_code           BS5024
_journal_date_accepted           2006-01-06
_journal_date_recd_electronic    2005-10-11
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              236
_journal_page_last               244
_journal_paper_category          FA
_journal_paper_doi               10.1107/S0108768106000802
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C21 H45 N3 Ni O3, F6 P, N O3'
_chemical_formula_sum            'C21 H45 F6 N4 Ni O6 P'
_chemical_formula_weight         653.29
_space_group_crystal_system      cubic
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_method           'XD routine XDCIF'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.008(2)
_cell_length_b                   14.008(2)
_cell_length_c                   14.008(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      2
_cell_volume                     2748.7(7)
_computing_cell_refinement       'Nonius CAD4 software, 1995'
_computing_data_collection       'Nonius CAD4 software, 1995'
_computing_data_reduction        'DREAR, Blessing, 1987'
_computing_molecular_graphics    'Ortep-3 for Windows, Farrugia 1997'
_computing_publication_material  'Koritsanszky et al, 2003'
_computing_structure_refinement  'Koritsanszky et al, 2003'
_computing_structure_solution    'SHELXS, Sheldrick, 1993'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'profile fitted \q/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       1
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20445
_diffrn_reflns_theta_full        49.93
_diffrn_reflns_theta_max         49.93
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0.5
_diffrn_standards_interval_time  120
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.804
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 ABSORB - DeTitta, G. Medical Foundation, Buffalo, 1984
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.579
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.236
_refine_ls_extinction_coef       0.67(5)
_refine_ls_extinction_expression
;
        Becker, P.J. & Coppens, P. (1974) Acta Cryst., A30, 129-153.
;
_refine_ls_extinction_method     'Becker-Coppens type 1 Lorentzian isotropic'
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         5095
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0219
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
        calc w1 = 1/[s^2^(Fo)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0152
_reflns_number_gt                5095
_reflns_number_total             6017
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bs5024.cif
_cod_data_source_block           multipole
_cod_depositor_comments
;
 Marking atom 'DUM0' as a dummy atom.

 Antanas Vaitkus,
 2017-02-19

 Adding the _atom_site_type_symbol data item.

 Antanas Vaitkus,
 2017-02-19

The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2100424