Co-Crystallized (Macrocyclic tetraamine)bis(thiocyanato-<i>N</i>)nickel(II) Complexes
Choi, Ki Young; Kim, Dong Won; Kim, Kyung-Han; Oh, Mi-Ran; Suh, Il-Hwan; Acta Crystallographica Section C 54 (1998) 627–628; doi:10.1107/S0108270197017368

data_2007209
_publ_section_title
;
 Co-Crystallized (Macrocyclic
 tetraamine)bis(thiocyanato-<i>N</i>)nickel(II) Complexes
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              627
_journal_page_last               628
_journal_paper_doi               10.1107/S0108270197017368
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          'Ni(NCS)~2~(C14 H32 N4)2 , C2 H3 N'
_chemical_formula_moiety         'C16 H32 N6 Ni S2 , C2 H3 N'
_chemical_formula_sum            'C18 H35 N7 Ni S2'
_chemical_formula_weight         472.34
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.81(2)
_cell_angle_beta                 91.18(2)
_cell_angle_gamma                104.910(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9990(10)
_cell_length_b                   13.867(2)
_cell_length_c                   8.911(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    288(2)
_cell_measurement_theta_max      14.1
_cell_measurement_theta_min      11.35
_cell_volume                     1193.5(6)
_computing_cell_refinement       SDP
_computing_data_collection       SDP_(Frenz,_1985)
_computing_data_reduction        SDP
_computing_molecular_graphics
ORTEP_(Johnson,_1976)_in_NRCVAX_(Gabe_et_al.,_1989)
_computing_publication_material  NRCVAX
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      288(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0650
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4374
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.005
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Block_cut_from_a_larger_crystal
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.66
_refine_diff_density_min         -0.39
_refine_ls_extinction_coef       none
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.270
_refine_ls_goodness_of_fit_obs   1.438
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         4183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.270
_refine_ls_restrained_S_obs      1.438
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_obs          .0583
_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^)+(0.02P)^2^+0.40P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1073
_refine_ls_wR_factor_obs         .0936
_reflns_number_observed          2576
_reflns_number_total             4183
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm1168.cif
_cod_data_source_block           real5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (10
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29 (8 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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^)+(0.02P)^2^+0.40P] 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^)+(0.02P)^2^+0.40P] where P=(Fo^2^+2Fc^2^)/3'.

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

2017-05-17
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C16 H32 N6 Ni S2) , 2(C2 H3 N)'
_cod_original_formula_iupac      '2[Ni(NCS)~2~(C14 H32 N4)2] , 2C2 H3 N'
_cod_original_formula_sum        'C36 H70 N14 Ni2 S4'
_cod_original_formula_units_Z    1
_cod_original_formula_weight     944.69
_cod_database_code               2007209