Acetonitriledichloro(1,4,7-triazacyclodecane)cobalt(III) perchlorate
Guo, Hui; Ren Yan-Wei; Li, Jun; Zhang, Feng-Xing; Acta Crystallographica Section E 61 (2005) m1080–m1081; doi:10.1107/S1600536805014042

data_2205865
_publ_section_title
;
 Acetonitriledichloro(1,4,7-triazacyclodecane)cobalt(III) perchlorate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1080
_journal_page_last               m1081
_journal_paper_doi               10.1107/S1600536805014042
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Co Cl2 (C7 H17 N3) (C2 H3 N)] Cl O4'
_chemical_formula_moiety         'C9 H20 Cl2 Co N4 +, Cl O4 -'
_chemical_formula_sum            'C9 H20 Cl3 Co N4 O4'
_chemical_formula_weight         413.57
_chemical_name_systematic
;
Acetonitriledichloro(1,4,7-triazacyclodecane)cobalt(III) perchlorate
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.863(4)
_cell_length_b                   10.7899(19)
_cell_length_c                   7.3630(13)
_cell_measurement_reflns_used    1445
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      23.58
_cell_measurement_theta_min      2.72
_cell_volume                     1657.5(5)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       \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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10135
_diffrn_reflns_theta_full        28.74
_diffrn_reflns_theta_max         28.74
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.537
_exptl_absorpt_correction_T_max  0.9553
_exptl_absorpt_correction_T_min  0.7345
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0583P)^2^+0.6755P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                1526
_reflns_number_total             2199
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6641.cif
_cod_data_source_block           I
_cod_database_code               2205865