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_2240776
_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          '[Cu (C4 N3) (C8 H20 N4)] (C4 N3)'
_chemical_formula_moiety         'C16 H20 Cu N10'
_chemical_formula_sum            'C16 H20 Cu N10'
_chemical_formula_weight         415.96
_chemical_name_systematic
'(1,4,7,10-Tetraazacyclododecane-\k^4^<i>N</i>)(tricyanomethanido-\k<i>N</i>)copper tricyanomethanide'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                89.187(3)
_cell_angle_beta                 88.236(3)
_cell_angle_gamma                78.579(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4074(15)
_cell_length_b                   11.552(2)
_cell_length_c                   11.625(2)
_cell_measurement_reflns_used    3012
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.17
_cell_measurement_theta_min      2.50
_cell_volume                     974.6(3)
_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 0.983
_diffrn_measured_fraction_theta_max 0.982
_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  0.0205
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.228
_diffrn_reflns_theta_min         1.798
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 1996)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.303
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4267
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.4093P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0884
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                3639
_reflns_number_total             4267
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5461sup1.cif
_cod_data_source_block           II
_cod_database_code               2240776
_cod_database_fobs_code          2240776
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.935
_shelx_hkl_checksum              82166
_shelx_res_checksum              20196
_shelxl_version_number           20.13