Solution-State and Solid-State Structural Characterization of Complexes of a New Macrocyclic Ligand Containing the 1,5-Diazacyclooctane Subunit
Chuanjiang Hu; Thoi D. Nguyen; Paul S. Wagenknecht; Lawrence C. Nathan; Inorganic Chemistry 42 (2003) 742–749; doi:10.1021/ic020495o

data_4313019
_publ_section_title
;
 Solution-State and Solid-State Structural Characterization of Complexes
 of a New Macrocyclic Ligand Containing the 1,5-Diazacyclooctane Subunit
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              742
_journal_page_last               749
_journal_paper_doi               10.1021/ic020495o
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C15 H28 Co N6 S2, C F3 O3 S'
_chemical_formula_sum            'C16 H28 Co F3 N6 O3 S3'
_chemical_formula_weight         564.55
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 109.165(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.230(3)
_cell_length_b                   11.446(2)
_cell_length_c                   16.238(2)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    298
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.83
_cell_volume                     2322.6(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      298
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       '\w scans'
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5042
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        3.8%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.879
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'Siemens SHELXTL'
_exptl_crystal_colour            'ruby red'
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.165
_refine_ls_extinction_coef       0.0038(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3994
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0624
_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^)+(0.1231P)^2^+6.0776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                2541
_reflns_number_total             4008
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020495o_2.cif
_cod_data_source_block           coc3cy
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313019