Structural relations in (1:1) and (2:1) Cyanobenzene-Ethylenedithio-TTF radical salts; The role of C≡N…H interactions.
Lopes, Gonçalo; Gama, Vasco Pires Silva da; Simão, Dulce; Santos, Isabel Cordeiro; Branco Lopes, Elsa; Pereira, Laura C. J.; Almeida, Manuel; Rabaça, Sandra; CrystEngComm  (2019) –; doi:10.1039/C9CE01214A

data_7234955
_publ_section_title
;
 Structural relations in (1:1) and (2:1) Cyanobenzene-Ethylenedithio-TTF
 radical salts; The role of C\\tb N&#x2026;H interactions.
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C9CE01214A
_journal_year                    2019
_chemical_formula_sum            'C34 H14 N6 Ni S16'
_chemical_formula_weight         1078.18
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc236jhc
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-02 deposited with the CCDC.	2019-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                98.5220(10)
_cell_angle_beta                 92.3060(10)
_cell_angle_gamma                100.265(2)
_cell_formula_units_Z            1
_cell_length_a                   7.1297(3)
_cell_length_b                   11.6789(4)
_cell_length_c                   12.4910(4)
_cell_measurement_reflns_used    3546
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.15
_cell_measurement_theta_min      2.62
_cell_volume                     1009.77(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury Macrae et al,2008)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9243
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.679
_diffrn_reflns_theta_min         2.910
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.347
_exptl_absorpt_correction_T_max  0.9736
_exptl_absorpt_correction_T_min  0.5524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_description       needle
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.0312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3187
_reflns_number_total             3821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01214a3.cif
_cod_data_source_block           (4-CNB-EDT-TTF)2[Ni(mnt)2]
_cod_original_cell_volume        1009.76(6)
_cod_database_code               7234955
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.552
_shelx_estimated_absorpt_t_max   0.974
_shelx_res_checksum              87333