Synthesis, characterization and crystal structures of mono and dinuclear macrocyclic cobalt(ii) complexes with a new tetraaza m-xylyl-based macrocyclic ligand
Khandar, Ali Akbar; Kirschbaum, Kristin; Abedi, Marjan; Mock, Kristi; Tracy, Greg; Spasojevic, Vojislav; Hosseini-Yazdi, Seyed Abolfazl; New J. Chem. 39 (2015) 2822–; doi:10.1039/C4NJ01608D

data_7054644
_publ_section_title
;
 Synthesis, characterization and crystal structures of mono and dinuclear
 macrocyclic cobalt(ii) complexes with a new tetraaza m-xylyl-based
 macrocyclic ligand
;
_journal_issue                   4
_journal_name_full               'New J. Chem.'
_journal_page_first              2822
_journal_paper_doi               10.1039/C4NJ01608D
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C22 H36 N4, 2(H2 O), 4(Cl)'
_chemical_formula_sum            'C22 H40 Cl4 N4 O2'
_chemical_formula_weight         534.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-01-23 deposited with the CCDC.
2015-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                62.925(3)
_cell_angle_beta                 67.443(3)
_cell_angle_gamma                69.428(4)
_cell_formula_units_Z            1
_cell_length_a                   7.9236(12)
_cell_length_b                   10.1680(17)
_cell_length_c                   10.2931(18)
_cell_measurement_reflns_used    4286
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      30.6
_cell_measurement_theta_min      2.7
_cell_volume                     665.97(19)
_computing_cell_refinement       'Bruker SAINT, V6.45A, 2003 '
_computing_data_collection       'Bruker SMART, 1997'
_computing_data_reduction        'Bruker SAINT, V6.45A, 2003'
_computing_molecular_graphics    'Diamond 2.0'
_computing_publication_material  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 6.14, 1998'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.847
_diffrn_measurement_device_type  'CCD detector Smart6000'
_diffrn_measurement_method       omega-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0220
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.847
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10396
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.847
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.057
_diffrn_reflns_theta_min         2.587
_exptl_absorpt_coefficient_mu    0.470
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Sheldrick1996;Blessing,ActaC.1995,A51,33
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       'parallel pipet'
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     225
_refine_ls_number_reflns         3938
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.2531P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0918
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3459
_reflns_number_total             3938
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4nj01608d1.cif
_cod_data_source_block           '[LH4]Cl4.2H2O'
_cod_depositor_comments
'Adding full bibliography for 7054642--7054644.cif.'
_cod_database_code               7054644
_shelxl_version_number           2014/6
_shelx_res_checksum              11740