Crystal structures of (1,4,7,10-tetraazacyclododecane-κ^4^<i>N</i>)bis(tricyanomethanido-κ<i>N</i>)nickel and (1,4,7,10-tetraazacyclododecane-κ^4^<i>N</i>)(tricyanomethanido-κ<i>N</i>)copper tricyanomethanide
Luo, Jun; Zhang, Xin-Rong; Qiu, Li-Juan; Yang, Feng; Liu, Bao-Shu; Acta Crystallographica Section E 71 (2015) 693–697; doi:10.1107/S2056989015009524

data_2240775
_publ_section_title
;
 Crystal structures of
 (1,4,7,10-tetraazacyclododecane-\k^4^<i>N</i>)bis(tricyanomethanido-\k<i>N</i>)nickel
 and
 (1,4,7,10-tetraazacyclododecane-\k^4^<i>N</i>)(tricyanomethanido-\k<i>N</i>)copper
 tricyanomethanide
;
_journal_coeditor_code           SJ5461
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              693
_journal_page_last               697
_journal_paper_doi               10.1107/S2056989015009524
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (C4 N3)2 (C8 H20 N4)]'
_chemical_formula_moiety         'C16 H20 N10 Ni'
_chemical_formula_sum            'C16 H20 N10 Ni'
_chemical_formula_weight         411.13
_chemical_name_systematic
(1,4,7,10-Tetraazacyclododecane-\k^4^<i>N</i>)bis(tricyanomethanido-\k<i>N</i>)nickel
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 104.828(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6300(12)
_cell_length_b                   11.0150(12)
_cell_length_c                   17.1771(18)
_cell_measurement_reflns_used    3344
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.84
_cell_measurement_theta_min      2.45
_cell_volume                     1944.3(4)
_computing_cell_refinement
;
SAINT (Bruker, 2010)
;
_computing_data_collection
;
APEX2 (Bruker, 2010)
;
_computing_data_reduction
;
SAINT (Bruker, 2010)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12264
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.910
_diffrn_reflns_theta_min         1.982
_exptl_absorpt_coefficient_mu    1.021
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.053
_refine_diff_density_min         -0.666
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     259
_refine_ls_number_reflns         4611
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0525
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+3.2428P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1243
_refine_ls_wR_factor_ref         0.1360
_reflns_number_gt                3460
_reflns_number_total             4611
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5461sup1.cif
_cod_data_source_block           I
_cod_database_code               2240775
_cod_database_fobs_code          2240775
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.960
_shelx_hkl_checksum              83884
_shelx_res_checksum              50156
_shelxl_version_number           20.13