μ-Cyanido-1:2κ^2^<i>N</i>:<i>C</i>-tricyanido-2κ^3^<i>C</i>-(<i>rac</i>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-1κ^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')dinickel(II) <i>N</i>,<i>N</i>-dimethylformamide monosolvate hemihydrate
Jiang, Hai-Ming; Ng, Seik Weng; Acta Crystallographica Section E 66 (2010) m1467–; doi:10.1107/S1600536810042625

data_2227262
_publ_section_title
;
 \m-Cyanido-1:2\k^2^<i>N</i>:<i>C</i>-tricyanido-2\k^3^<i>C</i>-(<i>rac</i>-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-1\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')dinickel(II)
 <i>N</i>,<i>N</i>-dimethylformamide monosolvate hemihydrate
;
_journal_coeditor_code           BT5382
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1467
_journal_paper_doi               10.1107/S1600536810042625
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'[Ni2 (C N)4 (C16 H36 N4)], C3 H7 N O, 0.5H2 O'
_chemical_formula_moiety         'C20 H36 N8 Ni2, C3 H7 N O, 0.5H2 O'
_chemical_formula_sum            'C23 H44 N9 Ni2 O1.5'
_chemical_formula_weight         588.09
_chemical_name_systematic
;
\m-Cyanido-1:2\k^2^<i>N</i>:<i>C</i>-tricyanido-2\k^3^<i>C</i>-(<i>rac</i>-
5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane-
1\k^4^<i>N</i>,<i>N</i>',<i>N</i>'',<i>N</i>''')dinickel(II)
<i>N</i>,<i>N</i>-dimethylformamide monosolvate hemihydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.4680(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0122(5)
_cell_length_b                   10.2109(5)
_cell_length_c                   28.3246(15)
_cell_measurement_reflns_used    5065
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.8
_cell_measurement_theta_min      2.5
_cell_volume                     2894.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       '\f and \w'
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            14236
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.8249
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prim
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.554
_refine_diff_density_min         -0.391
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         6181
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.7079P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                4435
_reflns_number_total             6181
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5382.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C23 H44 N9 Ni2 O1.50'
_cod_database_code               2227262
_cod_database_fobs_code          2227262