[1-(3-Aminopropyl)-4,7-dithia-1-azacyclononane-κ^4^<i>N</i>,<i>N</i>',<i>S,S</i>']bis(dimethylformamide-κ<i>O</i>)nickel(II) bis(tetraphenylborate) acetonitrile disolvate
Blake, Alexander J.; Lippolis, Vito; Acta Crystallographica Section E 61 (2005) m207–m208; doi:10.1107/S1600536804033380

data_2205167
_publ_section_title
;[1-(3-Aminopropyl)-4,7-dithia-1-azacyclononane-\k^4^<i>N</i>,<i>N</i>',<i>S,S</i>']bis(dimethylformamide-\k<i>O</i>)nickel(II)
 bis(tetraphenylborate) acetonitrile disolvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m207
_journal_page_last               m208
_journal_paper_doi               10.1107/S1600536804033380
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac
'[Ni (C3 H7 N O)2 (C9 H20 N2 S2)] (C24 H20 B)2, 2C2 H3 N'
_chemical_formula_moiety
'C15 H34 N4 Ni O2 S2 2+, 2C24 H20 B -, 2C2 H3 N'
_chemical_formula_sum            'C67 H80 B2 N6 Ni O2 S2'
_chemical_formula_weight         1145.82
_chemical_name_systematic
;
[1-(3-Aminopropyl)-4,7-dithia-1-azacyclononane-
\k^4^N,N',S,S']bis(dimethylformamide-\kO)nickel(II)
bis(tetraphenylborate) acetonitrile disolvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.06(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.907(4)
_cell_length_b                   11.951(4)
_cell_length_c                   26.516(5)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34
_cell_measurement_theta_min      26
_cell_volume                     6183(3)
_computing_cell_refinement       STADI-4
_computing_data_collection       'STADI-4 (Stoe & Cie, 1996)'
_computing_data_reduction        'X-RED (Stoe & Cie, 1996)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'enCIFer (Allen et al., 2004) and PLATON'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'Stoe Stadi-4'
_diffrn_measurement_method       \w-\q
_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  0.040
_diffrn_reflns_av_sigmaI/netI    0.037
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            12472
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        'random variation +-5'
_diffrn_standards_interval_count 60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.741
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(X-RED; Stoe & Cie, 1996)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    none
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.25
_refine_diff_density_min         -0.73
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.05
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         10898
_refine_ls_number_restraints     709
_refine_ls_restrained_S_all      1.03
_refine_ls_R_factor_all          0.087
_refine_ls_R_factor_gt           0.069
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.122P)^2^+7.311P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.182
_refine_ls_wR_factor_ref         0.205
_reflns_number_observed          8397
_reflns_number_total             10898
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            tk6203.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2205167
_cod_database_fobs_code          2205167