The first structurally characterised perchlorato-cobalt(III) complexes, involving the C-bonded macrobicyclic ligand 1,4,8,11-tetraazabicyclo[9.5.2]octadecane
Zhou, Xiangting; Day, Anthony I.; Willis, Anthony C.; Jackson, W. Gregory; Chemical Communications (Cambridge, United Kingdom)  (2003) 2386–2387; doi:10.1039/b305182j

data_7104781
_publ_section_title
;
 The first structurally characterised perchlorato-cobalt(III)
 complexes, involving the C-bonded macrobicyclic ligand
 1,4,8,11-tetraazabicyclo[9.5.2]octadecane
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   18
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2386
_journal_page_last               2387
_journal_paper_doi               10.1039/b305182j
_journal_year                    2003
_chemical_absolute_configuration ad
_chemical_formula_moiety         ' C14 H29 Cl Co1 N4 O4 +, Cl O4 -'
_chemical_formula_sum            'C14 H29 Cl2 Co N4 O8'
_chemical_formula_weight         511.24
_chemical_melting_point          ?
_chemical_name_common            'Sym-anti perchlorato'
_chemical_name_systematic        'Sym-anti perchlorato'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             03-13-01
_audit_creation_method           CRYSTALS_ver_12-03-99
_audit_update_record
;
2003-01-14 - Report on C14 H29 Cl2 Co N4 O9  (S-D952-2)
by Anthony C. Willis
for W. Greg Jackson and Xiangting Zhou, ADFA
2003-01-14 - passes checkcif tests with minor warnings
;
_cell_angle_alpha                90.0
_cell_angle_beta                 108.442(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            2
_cell_length_a                   8.1097(1)
_cell_length_b                   14.6807(3)
_cell_length_c                   8.7957(2)
_cell_measurement_reflns_used    21669
_cell_measurement_temperature    200
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     993.40(3)
_computing_cell_refinement
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
teXsan (MSC, 1992-1997)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       ' \f and \w scans with CCD '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.07
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            24988
_diffrn_reflns_theta_full        30.01
_diffrn_reflns_theta_max         30.01
_diffrn_reflns_theta_min         4.13
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.185
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.704
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
via Gaussian method (Coppens, 1970) implemented in maXus (2000)
;
_exptl_crystal_colour            ' purple '
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             533.411
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.32
_refine_diff_density_min         -0.50
_refine_ls_abs_structure_details 'Flack, 2768 Friedel-pairs'
_refine_ls_abs_structure_Flack   0.004(16)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0641
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3703
_refine_ls_R_factor_gt           0.0368
_refine_ls_shift/su_max          0.016625
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Chebychev polynomial with 3 parameters, Carruthers & Watkin , 1979,
0.635    0.226    0.338
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0416
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              20
_reflns_limit_k_min              -20
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                3703
_reflns_number_total             5778
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            b305182j.txt
_cod_data_source_block           wgj11
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 21 1 '
_cod_original_formula_sum        ' C14 H29 Cl2 Co1 N4 O8 '
_cod_database_code               7104781