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_1567587
_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         'C70 H56 Co N10 O2 S2, 2(C H Cl3), 1[CHCl3]'
_chemical_formula_sum            'C73 H59 Cl9 Co N10 O2 S2'
_chemical_formula_weight         1550.40
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-05
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.944(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7142(9)
_cell_length_b                   9.8420(5)
_cell_length_c                   25.6400(17)
_cell_measurement_reflns_used    34675
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.80
_cell_measurement_theta_min      3.46
_cell_volume                     3699.3(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
 2037 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  0.0413
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            31869
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.075
_diffrn_reflns_theta_min         4.815
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.755
_exptl_absorpt_correction_T_max  0.2100
_exptl_absorpt_correction_T_min  0.1347
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1590
_exptl_crystal_recrystallization_method
'The material was recrystallised from a mixture of CHCl3 and methanol  by solvent layering'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.12
_exptl_crystal_size_rad          0.160
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.089
_refine_ls_extinction_coef       0.0026(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   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         7229
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0845
_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^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2057
_refine_ls_wR_factor_ref         0.2316
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5841
_reflns_number_total             7229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            NIA006_150K.cif
_cod_data_source_block           nia006_150k
_cod_database_code               1567587
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.545
_shelx_estimated_absorpt_t_min   0.392
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1-H1
 0.85 with sigma of 0.01
 Co1-H1
 2.644499 with sigma of 0.02
 C35-H1
 1.869092 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C34(H34)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C21(H21), C16(H16), C11(H11), C3(H3), C17(H17), C19(H19),
 C13(H13), C2(H2), C14(H14), C12(H12), C1(H1A), C23(H23), C29(H29), C20(H20),
 C33(H33), C30(H30), C25(H25), C24(H24), C31(H31), C27(H27), C26(H26), C32(H32)
3.c Idealised Me refined as rotating group:
 C35(H35A,H35B,H35C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              14145
_shelx_hkl_checksum              67220
_shelx_fab_checksum              44960
_olex2_date_sample_data_collection 2022-05-04
_olex2_date_sample_submission    2022-04-29
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id NIA006_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   7.2
_stoe_evaluation_integration_b   -1.0
_stoe_evaluation_integration_ems 0.016
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 4
_stoe_evaluation_lana_bos_l_odd_max 1
_stoe_evaluation_lana_completeness 97.9
_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 146.2
_stoe_evaluation_lana_max_2theta_desired 146.2
_stoe_evaluation_lana_mean_redundancy 4.4
_stoe_evaluation_lana_number_refls_after_or 31879
_stoe_evaluation_lana_number_refls_outliers 13447
_stoe_evaluation_lana_number_refls_total 45326
_stoe_evaluation_lana_number_refls_unique 7236
_stoe_evaluation_lana_number_refls_written 31879
_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          14.2   29.8   45.4   61.0   76.6   92.2  107.8  123.4  139.0
----------------------------------------------------------------------------
<Resolution>    5.14   2.85   1.97   1.49   1.24   1.07   0.95   0.88   0.83
N(total)         189   1194   2887   5854   9804  10041   6491   5830   3036
<Redundancy>     2.3    3.8    3.9    5.2    6.5    5.7    3.5    3.4    2.7
Complet. [%%]    91.7   98.2   99.4   99.9  100.0  100.0   99.8   99.9   86.2
<I/sigma>      350.9  213.7  107.2   44.1   26.0   14.9    9.7    5.5    2.3
R(int)         0.019  0.028  0.026  0.042  0.047  0.067  0.097  0.174  0.379
----------------------------------------------------------------------------
;
_stoe_measurement_identifier     NIA006_150K
_stoe_measurement_max_exposure_per_frame '12.0 s'
_stoe_measurement_mean_exposure_per_frame '11.2 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '6.3 h'
_stoe_measurement_total_frame_number 2037
_stoe_measurement_total_run_number 42
_stoe_measurement_tube_power     '50.0 W'