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_7054643
_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_absolute_configuration R,S
_chemical_formula_moiety         '[C22 H34 Cl2 Co N4][Cl]2'
_chemical_formula_sum            'C22 H34 Cl4 Co N4'
_chemical_formula_weight         555.26
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8736(2)
_cell_length_b                   13.6929(3)
_cell_length_c                   21.0647(6)
_cell_measurement_reflns_used    3978
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      2.4
_cell_volume                     2559.47(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.931
_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  0.0402
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            20953
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.902
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         33.449
_diffrn_reflns_theta_min         1.774
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.567
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS;Sheldrick1996;Blessing,ActaC.1995,A51,33
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       orthorhombic
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 2338 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         9030
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0850
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1336
_reflns_Friedel_coverage         0.748
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.866
_reflns_number_gt                6803
_reflns_number_total             9030
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4nj01608d1.cif
_cod_data_source_block           added_by_encifer
_cod_depositor_comments
'Adding full bibliography for 7054642--7054644.cif.'
_cod_database_code               7054643
_shelxl_version_number           2014/6
_shelx_res_checksum              33608