To Be or Not to Be a (4,4) Net: Reactions of 4′-{4-(N,N-Diethylaminophenyl)}- and 4′-{4-(N,N-Diphenylaminophenyl)}-3,2′:6′,3″- and 4,2′:6′,4″-Terpyridines with Cobalt(II) Thiocyanate
Rocco, Dalila; Nikoletić, Anamarija; Prescimone, Alessandro; Constable, Edwin C.; Housecroft, Catherine E.; Crystals 12 (2022) 1136–; doi:10.3390/cryst12081136

data_1567585
_publ_section_title
;
 To Be or Not to Be a (4,4) Net: Reactions of
 4&#x2032;-{4-(N,N-Diethylaminophenyl)}- and
 4&#x2032;-{4-(N,N-Diphenylaminophenyl)}-3,2&#x2032;:6&#x2032;,3&#x2033;-
 and 4,2&#x2032;:6&#x2032;,4&#x2033;-Terpyridines with Cobalt(II)
 Thiocyanate
;
_journal_issue                   8
_journal_name_full               Crystals
_journal_page_first              1136
_journal_paper_doi               10.3390/cryst12081136
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C68 H48 Co N10 S2'
_chemical_formula_sum            'C68 H48 Co N10 S2'
_chemical_formula_weight         1128.21
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-05-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.524(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.7148(3)
_cell_length_b                   18.4121(6)
_cell_length_c                   18.2547(5)
_cell_measurement_reflns_used    25516
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.92
_cell_measurement_theta_min      5.18
_cell_volume                     2870.06(16)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_detector_type            'DECTRIS EIGER2 1M'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
 1953 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.1661
_diffrn_reflns_av_unetI/netI     0.0610
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            58771
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.144
_diffrn_reflns_theta_min         4.945
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.430
_exptl_absorpt_correction_T_max  0.1992
_exptl_absorpt_correction_T_min  0.0792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.160
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.127
_refine_ls_extinction_coef       0.0025(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     368
_refine_ls_number_reflns         5669
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1614
_refine_ls_R_factor_gt           0.1458
_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^)+(0.1200P)^2^+30.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3652
_refine_ls_wR_factor_ref         0.3729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4410
_reflns_number_total             5669
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NIA026_150K.cif
_cod_data_source_block           nia026_150k
_cod_database_code               1567585
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.547
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C15(H15), C10(H10), C14(H14), C2(H2), C26(H26), C7(H7),
 C18(H18), C29(H29), C13(H13), C23(H23), C25(H25), C21(H21), C11(H11), C30(H30),
  C24(H24), C27(H27), C19(H19), C5(H5), C20(H20), C33(H33), C32(H32), C31(H31)
;
_shelx_res_checksum              14554
_shelx_hkl_checksum              75688
_olex2_date_sample_data_collection 2022-05-19
_olex2_date_sample_submission    2022-05-16
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id NIA026_150K
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   5.6
_stoe_evaluation_integration_b   -1.0
_stoe_evaluation_integration_ems 0.019
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 6
_stoe_evaluation_lana_bos_l_odd_max 3
_stoe_evaluation_lana_completeness 98.9
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 146.3
_stoe_evaluation_lana_max_2theta_desired 146.3
_stoe_evaluation_lana_mean_redundancy 4.5
_stoe_evaluation_lana_number_refls_after_or 51282
_stoe_evaluation_lana_number_refls_outliers 8754
_stoe_evaluation_lana_number_refls_total 60036
_stoe_evaluation_lana_number_refls_unique 11421
_stoe_evaluation_lana_number_refls_written 58974
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group 2/m
_stoe_evaluation_lana_table
;
--------------------------------------
2Theta          12.4   28.2   44.0   59.8   75.6   91.4  107.2  123.0  138.8
--------------------------------------
<Resolution>    5.76   2.93   2.03   1.51   1.25   1.08   0.95   0.88   0.83
N(total)          47   1138   2805   6745  12889  14031   9429   8703   4249
<Redundancy>     1.2    2.8    3.1    4.3    6.3    5.9    4.0    4.0    2.9
Complet. [%%]    81.3   97.0  100.0  100.0  100.0  100.0   99.9  100.0   93.5
<I/sigma>      167.6   68.1   36.7   13.3    7.5    4.9    2.8    1.5    1.0
R(int)         0.006  0.024  0.026  0.058  0.077  0.089  0.158  0.238  0.315
--------------------------------------
;
_stoe_measurement_identifier     NIA026_150K
_stoe_measurement_max_exposure_per_frame '15.0 s'
_stoe_measurement_mean_exposure_per_frame '14.6 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '7.9 h'
_stoe_measurement_total_frame_number 1953
_stoe_measurement_total_run_number 34
_stoe_measurement_tube_power     '50.0 W'