Crystal structures of 5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane cobalt(III) mono-phenylacetylide and bis-phenylacetylide
Oxley, Benjamin M.; Mash, Brandon; Zeller, Matthias; Banziger, Susannah; Ren, Tong; Acta Crystallographica Section E 74 (2018) 522–529; doi:10.1107/S2056989018003997

data_2242427
_publ_section_title
;
 Crystal structures of 5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane
 cobalt(III) mono-phenylacetylide and bis-phenylacetylide
;
_journal_coeditor_code           VM2209
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              522
_journal_page_last               529
_journal_paper_doi               10.1107/S2056989018003997
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac
'[Co (C8 H5) Cl (C12 H28 N4)] Cl, C2 H3 N, C H4 O'
_chemical_formula_moiety         'C20 H33 Cl Co N4 +, Cl -, C2 H3 N, C H4 O'
_chemical_formula_sum            'C23 H40 Cl2 Co N5 O'
_chemical_formula_weight         532.43
_chemical_name_systematic
'Chlorido(5,12-dimethyl-1,4,8,11-tetraazacyclotetradecane)(phenylethynyl)cobalt(III) chloride--acetonitrile--methanol (1/1/1)'
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                86.430(5)
_cell_angle_beta                 74.848(4)
_cell_angle_gamma                88.970(5)
_cell_formula_units_Z            4
_cell_length_a                   9.6903(13)
_cell_length_b                   15.668(2)
_cell_length_c                   17.985(2)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.3695
_cell_measurement_theta_min      3.0510
_cell_volume                     2630.6(6)
_computing_cell_refinement
;
SAINT (Bruker, 2016)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2016)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015) and
<i>SHELXLE</i> (H\"ubschle <i>et al.</i>,  2011)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44192
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.987
_exptl_absorpt_coefficient_mu    0.880
_exptl_absorpt_correction_T_max  0.2627
_exptl_absorpt_correction_T_min  0.1896
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       plate
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.090
_refine_diff_density_max         0.927
_refine_diff_density_min         -1.405
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         9687
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1142
_refine_ls_R_factor_gt           0.0867
_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^)+(0.0698P)^2^+11.8383P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2119
_refine_ls_wR_factor_ref         0.2410
_reflns_number_gt                7643
_reflns_number_total             9687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2209sup1.cif
_cod_data_source_block           1
_cod_database_code               2242427
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.925
_shelx_hkl_checksum              11785
_shelx_res_checksum              48186
_cod_database_fobs_code 2242427