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_2242428
_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
'2[Co (C8 H5)2 (C12 H28 N4)] (C F3 S O3)2, C H2 Cl2'
_chemical_formula_moiety
'2(C28 H38 Co N4 +), 2(C F3 O3 S -), C H2 Cl2'
_chemical_formula_sum            'C59 H78 Cl2 Co2 F6 N8 O6 S2'
_chemical_formula_weight         1362.17
_chemical_name_systematic
'(5,12-Dimethyl-1,4,8,11-tetraazacyclotetradecane)bis(phenylethynyl)cobalt(III) trifluoromethanesulfonate--dichloromethane (2/1)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 105.3260(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0263(7)
_cell_length_b                   12.3999(5)
_cell_length_c                   21.9164(14)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.9243
_cell_measurement_theta_min      3.2855
_cell_volume                     3152.1(3)
_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
;
SHELXL2018 (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 0.996
_diffrn_measured_fraction_theta_max 0.990
_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  0.0259
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            54456
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.206
_diffrn_reflns_theta_min         2.891
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6600
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.557
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 6987 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.003(3)
_refine_ls_extinction_coef       0.0043(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     872
_refine_ls_number_reflns         22462
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0340
_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^)+(0.0368P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0779
_reflns_number_gt                18066
_reflns_number_total             22462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vm2209sup1.cif
_cod_data_source_block           2
_cod_database_code               2242428
_shelx_estimated_absorpt_t_min   0.753
_shelx_estimated_absorpt_t_max   0.929
_shelx_hkl_checksum              69074
_shelx_res_checksum              90842
_cod_database_fobs_code 2242428