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_1567589
_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         'C33 H24 N4'
_chemical_formula_sum            'C33 H24 N4'
_chemical_formula_weight         476.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 146.585(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   34.855(5)
_cell_length_b                   8.6116(8)
_cell_length_c                   30.178(5)
_cell_measurement_reflns_used    10443
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.88
_cell_measurement_theta_min      4.59
_cell_volume                     4988.3(15)
_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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
 3613 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  Basel-Cu-Stoe
_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  0.0744
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            36601
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         67.998
_diffrn_reflns_theta_min         4.607
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.589
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_correction_T_min  0.9743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.150
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0024(3)
_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   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1376
_refine_ls_R_factor_gt           0.0975
_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^)+(0.1000P)^2^+27.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2194
_refine_ls_wR_factor_ref         0.2699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3249
_reflns_number_total             4524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NIA002_150K.cif
_cod_data_source_block           nia002_150k
_cod_original_cell_volume        4988.2(12)
_cod_database_code               1567589
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.891
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C24(H24), C14(H14), C9(H9), C23(H23), C6(H6), C13(H13), C3(H3), C10(H10),
 C12(H12), C2(H2), C26(H26), C21(H21), C25(H25), C29(H29), C27(H27), C1(H1),
 C17(H17), C30(H30), C20(H20), C33(H33), C18(H18), C19(H19), C31(H31), C32(H32)
;
_shelx_res_checksum              67153
_shelx_hkl_checksum              39009
_olex2_date_sample_data_collection 2022-04-28
_olex2_date_sample_submission    2022-04-22
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id NIA002_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 0.020
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max -
_stoe_evaluation_lana_bos_l_odd_max -
_stoe_evaluation_lana_completeness 99.7
_stoe_evaluation_lana_dxs_max_order -
_stoe_evaluation_lana_dys_max_order -
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 147.6
_stoe_evaluation_lana_max_2theta_desired 136.0
_stoe_evaluation_lana_mean_redundancy 8.1
_stoe_evaluation_lana_number_refls_after_or 36616
_stoe_evaluation_lana_number_refls_outliers 13279
_stoe_evaluation_lana_number_refls_total 49895
_stoe_evaluation_lana_number_refls_unique 4534
_stoe_evaluation_lana_number_refls_written 36616
_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          12.2   26.8   41.4   56.0   70.6   85.2   99.8  114.4  129.0
----------------------------------------------------------------------------
<Resolution>    6.01   3.06   2.14   1.60   1.33   1.14   1.01   0.92   0.86
N(total)          21    686   1994   4026   9475  11242   8538   7845   6068
<Redundancy>     1.3    3.8    4.9    6.4   11.3   11.0    7.7    7.4    6.8
Complet. [%%]    57.7   99.2  100.0  100.0  100.0  100.0   99.9   99.9  100.0
<I/sigma>       74.8  104.8   51.8   23.0   12.8   11.8    7.1    2.8    1.0
R(int)         0.298  0.055  0.042  0.052  0.077  0.071  0.115  0.290  0.524
----------------------------------------------------------------------------
;
_stoe_measurement_identifier     NIA002_150K
_stoe_measurement_max_exposure_per_frame '10.0 s'
_stoe_measurement_mean_exposure_per_frame '10.0 s'
_stoe_measurement_min_exposure_per_frame '10.0 s'
_stoe_measurement_total_exposure_time '10.0 h'
_stoe_measurement_total_frame_number 3613
_stoe_measurement_total_run_number 58
_stoe_measurement_tube_power     '50.0 W'