Crystal structure and spectroscopic characterization of a cobalt(II) tetraazamacrocycle: completing a series of first-row transition-metal complexes
Van Heuvelen, Katherine M.; Lee, Isabell; Arriola, Katherine; Griffin, Rilke; Ye, Christopher; Takase, Michael K.; Acta Crystallographica Section C 73 (2017) –; doi:10.1107/S2053229617010397

data_2020757
_publ_section_title
;
 Crystal structure and spectroscopic characterization of a cobalt(II)
 tetraazamacrocycle: completing a series of first-row transition-metal
 complexes
;
_journal_coeditor_code           YP3138
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229617010397
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Co Cl (C14 H32 N4)] Cl, 2H2 O'
_chemical_formula_moiety         'C14 H32 Cl Co N4 +, Cl -, 2(H2 O)'
_chemical_formula_sum            'C14 H36 Cl2 Co N4 O2'
_chemical_formula_weight         422.30
_chemical_name_systematic
'Chlorido(1,4,8,11-tetramethyl-1,4,8,11-tetraazacyclotetradecane-\k^4^<i>N</i>)cobalt(II) chloride dihydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90.735(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2864(8)
_cell_length_b                   17.0679(16)
_cell_length_c                   13.9733(14)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.84
_cell_measurement_theta_min      2.46
_cell_volume                     1976.1(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2017)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 VENTURE Kappa Duo PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            72258
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.368
_diffrn_reflns_theta_min         2.458
_exptl_absorpt_coefficient_mu    1.152
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.563
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         9577
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0244P)^2^+0.7824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0655
_reflns_number_gt                7769
_reflns_number_total             9577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3138sup1.cif
_cod_data_source_block           I
_cod_database_code               2020757
_shelx_estimated_absorpt_t_min   0.656
_shelx_estimated_absorpt_t_max   0.762
_shelx_hkl_checksum              58830
_shelx_res_checksum              58884
_cod_database_fobs_code 2020757