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_7058600
_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         'C26 H24 N2 Ni O4 S6, C3 H7 N O'
_chemical_formula_sum            'C29 H31 N3 Ni O5 S6'
_chemical_formula_weight         752.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 108.2360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6638(2)
_cell_length_b                   8.31590(10)
_cell_length_c                   23.1526(2)
_cell_measurement_reflns_used    8780
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.8220
_cell_measurement_theta_min      1.7070
_cell_volume                     3230.09(6)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Elettra XRD1 data collection SW'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f      0.00 180.00   1.00    3.00   0.00   0.00   0.00    --   180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Huber 4-circles K goniometer, Pilatus 2M detector'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0411321000
_diffrn_orient_matrix_UB_12      -0.0088880000
_diffrn_orient_matrix_UB_13      0.0058650000
_diffrn_orient_matrix_UB_21      -0.0058153000
_diffrn_orient_matrix_UB_22      -0.0071930000
_diffrn_orient_matrix_UB_23      -0.0312105000
_diffrn_orient_matrix_UB_31      0.0038710000
_diffrn_orient_matrix_UB_32      0.0834071000
_diffrn_orient_matrix_UB_33      -0.0020780000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.954
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            16441
_diffrn_reflns_point_group_measured_fraction_full 0.954
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        24.623
_diffrn_reflns_theta_max         24.623
_diffrn_reflns_theta_min         1.716
_diffrn_source                   'Elettra synchrotron XRD1 BL'
_exptl_absorpt_coefficient_mu    0.993
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             1560
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.436
_refine_diff_density_min         -1.253
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.002
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1238
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4912
_reflns_number_total             5438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj02976a2.cif
_cod_data_source_block           4_niddd115_1_
_cod_depositor_comments
'Adding full bibliography for 7058598--7058600.cif.'
_cod_database_code               7058600
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 76.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.00
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C41(H41A,H41B), C51(H51A,H51B), C121(H12A,H12B)
2.b Aromatic/amide H refined with riding coordinates:
 C111(H111), C71(H71), C81(H81), C101(H101), C91(H91), C181(H181), C141(H141),
 C171(H171), C151(H151), C161(H161), C1S(H1S)
2.c Idealised Me refined as rotating group:
 C62(H62A,H62B,H62C), C82(H82A,H82B,H82C), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,
 H3SC)
;
_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.705