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_1512411
_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_sum            'C44 H52 Co2 Mn N20 O8'
_chemical_formula_weight         1161.86
_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                79.728(5)
_cell_angle_beta                 70.235(4)
_cell_angle_gamma                73.535(5)
_cell_formula_units_Z            1
_cell_length_a                   9.847(3)
_cell_length_b                   11.660(4)
_cell_length_c                   12.169(4)
_cell_measurement_reflns_used    2484
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      2.44
_cell_volume                     1255.7(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6326
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.974
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.642188
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             599
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         4396
_refine_ls_number_restraints     52
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0939P)^2^+1.2784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1804
_reflns_number_gt                3056
_reflns_number_total             4396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-390-178-183-1.cif
_cod_data_source_block           060929a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to the built-in table from CIF Core dictionary
named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_hydrogen_treatment' value 'CONSTR' changed
to 'constr' 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 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1255.6(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1512411