Synthesis and crystal structures of the first cobalt complexes of macrocyclic oxamido
Rui-hong Zhang; Qing-lun Wang; Guang-ming Yang; Inorganica Chimica Acta 390 (2012) 178–183; doi:10.1016/j.ica.2012.04.022

data_1512414
_publ_section_title
;
 Synthesis and crystal structures of the first cobalt complexes of
 macrocyclic oxamido
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              178
_journal_page_last               183
_journal_paper_doi               10.1016/j.ica.2012.04.022
_journal_volume                  390
_journal_year                    2012
_chemical_formula_moiety         'C20 H21 Co1.50 N10 O3'
_chemical_formula_sum            'C20 H21 Co1.5 N10 O3'
_chemical_formula_weight         537.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.978(5)
_cell_angle_beta                 96.321(6)
_cell_angle_gamma                104.489(7)
_cell_formula_units_Z            2
_cell_length_a                   8.580(4)
_cell_length_b                   9.636(4)
_cell_length_c                   13.281(6)
_cell_measurement_reflns_used    2869
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.2
_cell_volume                     1040.7(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'Rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13147
_diffrn_reflns_theta_full        27.89
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.8844
_exptl_absorpt_correction_T_min  0.8051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.716
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             551
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.927
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+2.0763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                3921
_reflns_number_total             4936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-390-178-183-4.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        1040.8(8)
_cod_original_formula_sum        'C20 H21 Co1.50 N10 O3'
_cod_database_code               1512414