Design of nickel donor‒acceptor dithiolenes for 2nd order nonlinear optics: an experimental and computational study
Attar, Salahuddin S.; Marchiò, Luciano; Pilia, Luca; Casula, Maria F.; Espa, Davide; Serpe, Angela; Pizzotti, Maddalena; Marinotto, Daniele; Deplano, Paola; New Journal of Chemistry 43 (2019) 12570–; doi:10.1039/C9NJ02976A

data_7058598
_publ_section_title
;
 Design of nickel donor--acceptor dithiolenes for 2nd order nonlinear
 optics: an experimental and computational study
;
_journal_issue                   32
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12570
_journal_paper_doi               10.1039/C9NJ02976A
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         'C22 H18 N4 Ni S4'
_chemical_formula_sum            'C22 H18 N4 Ni S4'
_chemical_formula_weight         525.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-16 deposited with the CCDC.    2019-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                73.582(4)
_cell_angle_beta                 70.444(5)
_cell_angle_gamma                83.313(5)
_cell_formula_units_Z            2
_cell_length_a                   9.040(3)
_cell_length_b                   11.556(3)
_cell_length_c                   12.136(4)
_cell_measurement_reflns_used    4328
_cell_measurement_temperature    296
_cell_measurement_theta_max      24.404
_cell_measurement_theta_min      2.240
_cell_volume                     1145.6(6)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       Smart
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker Smart Breeze'
_diffrn_measurement_method       'omega and phi scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12122
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.825
_diffrn_reflns_theta_max         24.825
_diffrn_reflns_theta_min         1.838
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6195
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1166 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.8314.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear dark black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       prism
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.255
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         3935
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0418P)^2^+0.2650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3258
_reflns_number_total             3935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02976a2.cif
_cod_data_source_block           1_nimnt115
_cod_depositor_comments
'Adding full bibliography for 7058598--7058600.cif.'
_cod_database_code               7058598
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N11-C31A = N11-C31 = N21-C41A = N21-C41 = C31A-C41A = C31-C41
 1.5 with sigma of 0.02
3. Others
 Sof(C31)=Sof(H31C)=Sof(H31D)=Sof(C41)=Sof(H41C)=Sof(H41D)=1-FVAR(1)
 Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C31A)=Sof(H31A)=Sof(H31B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C121(H12A,H12B), C41A(H41A,H41B), C31A(H31A,H31B), C31(H31C,
 H31D), C41(H41C,H41D)
4.b Aromatic/amide H refined with riding coordinates:
 C71(H71), C81(H81), C91(H91), C101(H101), C111(H111), C181(H181), C171(H171),
 C161(H161), C151(H151), C141(H141)
;
_olex2_submission_special_instructions 'No special instructions were received'