μ-1,5-Dicyanamido-bis[chloro(1,4,7-triazacyclononane)copper(II)] perchlorate
Zhao-Dong Wang; Wei Han; Shi-Ping Yan; Dai-Zheng Liao; Zong-Hui Jiang; Peng Cheng; Acta Crystallographica Section E 60 (2004) m1137–m1138; doi:10.1107/S1600536804017076

data_2204068
_publ_section_title
;
 \m-1,5-Dicyanamido-bis[chloro(1,4,7-triazacyclononane)copper(II)]
 perchlorate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1137
_journal_page_last               m1138
_journal_paper_doi               10.1107/S1600536804017076
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Cu2 (C2 N3) Cl2 (C6 H15 N3)2] Cl O4'
_chemical_formula_moiety         'C14 H30 Cl2 Cu2 N9 +, Cl O4 -'
_chemical_formula_sum            'C14 H30 Cl3 Cu2 N9 O4'
_chemical_formula_weight         621.90
_chemical_name_systematic
;
\m-1,5-Dicyanamido-bis[chloro(1,4,7-triazacyclononane)copper(II)] perchlorate
;
_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                90.00
_cell_angle_beta                 105.200(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.882(6)
_cell_length_b                   7.494(3)
_cell_length_c                   18.596(6)
_cell_measurement_reflns_used    864
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      2.27
_cell_volume                     2404.8(15)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13116
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    2.142
_exptl_absorpt_correction_T_max  0.773
_exptl_absorpt_correction_T_min  0.592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.418
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         4901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0776
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.6189P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                3372
_reflns_number_total             4901
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6384.cif
_cod_data_source_block           I
_cod_original_cell_volume        2404.9(14)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2204068
_cod_database_fobs_code          2204068