Schiff-base [4]helicene Zn(II) complexes as chiral emitters.
Savchuk, Mariia; Vertueux, Steven; Cauchy, Thomas; Loumaigne, Matthieu; Zinna, Francesco; Di Bari, Lorenzo; Zigon, Nicolas; Avarvari, Narcis; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10533–10539; doi:10.1039/d1dt01752g

data_7707783
_publ_section_title
;
 Schiff-base [4]helicene Zn(II) complexes as chiral emitters.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10533
_journal_page_last               10539
_journal_paper_doi               10.1039/d1dt01752g
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C19 H11 N O, C H4 O'
_chemical_formula_sum            'C20 H15 N O2'
_chemical_formula_weight         301.33
_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'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-26
_audit_creation_method           SHELXL2018/3
_audit_update_record
;
2021-04-29 deposited with the CCDC.	2021-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.0
_cell_angle_beta                 109.066(2)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   10.7403(2)
_cell_length_b                   10.84250(16)
_cell_length_c                   13.7128(3)
_cell_measurement_reflns_used    6556
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      76.1990
_cell_measurement_theta_min      4.3190
_cell_volume                     1509.28(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1990
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -62.00  32.00   1.00    1.00    --  -43.24  19.00  90.00   94
  2  \w      5.00  34.00   1.00    1.00    --   43.24-125.00-150.00   29
  3  \w     31.00 108.00   1.00    2.97    --  111.00 -94.00 -90.00   77
  4  \w     89.00 116.00   1.00    2.97    --  111.00 -61.00 -90.00   27
  5  \w     76.00 125.00   1.00    2.97    --  111.00 -30.00 -90.00   49
  6  \w    122.00 156.00   1.00    2.97    --  111.00  45.00   0.00   34
  7  \w    127.00 156.00   1.00    2.97    --  111.00  77.00   0.00   29
  8  \w    131.00 156.00   1.00    2.97    --  111.00  77.00  60.00   25
  9  \w    120.00 155.00   1.00    2.97    --  111.00  30.00  90.00   35
 10  \w     95.00 158.00   1.00    2.97    --  111.00  61.00 -30.00   63
 11  \w    126.00 153.00   1.00    2.97    --  111.00  45.00 -60.00   27
 12  \w    120.00 151.00   1.00    2.97    --  111.00  45.00-150.00   31
 13  \w     99.00 134.00   1.00    2.97    --  111.00  45.00-180.00   35
 14  \w     90.00 115.00   1.00    2.97    --  111.00  45.00-150.00   25
 15  \w     99.00 124.00   1.00    2.97    --  111.00  45.00 -90.00   25
 16  \w     99.00 152.00   1.00    2.97    --  111.00  77.00 -60.00   53
 17  \w     92.00 117.00   1.00    2.97    --  111.00  45.00 -60.00   25
 18  \w     97.00 129.00   1.00    2.97    --  111.00 125.00-120.00   32
 19  \w     86.00 145.00   1.00    2.97    --  111.00  77.00  90.00   59
 20  \w     90.00 126.00   1.00    2.97    --  111.00  45.00 150.00   36
 21  \w     66.00 108.00   1.00    2.97    --  111.00 -94.00 -30.00   42
 22  \w     47.00  72.00   1.00    2.97    --  111.00 -61.00 -90.00   25
 23  \w     37.00  74.00   1.00    2.97    --  111.00 -94.00-120.00   37
 24  \w     40.00  66.00   1.00    2.97    --  111.00-125.00-180.00   26
 25  \w   -113.00 -21.00   1.00    1.00    --  -43.24 -38.00 -90.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova (Cu) X-ray Source'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1247159000
_diffrn_orient_matrix_UB_12      -0.0808611000
_diffrn_orient_matrix_UB_13      -0.0349622000
_diffrn_orient_matrix_UB_21      -0.0681872000
_diffrn_orient_matrix_UB_22      0.0879040000
_diffrn_orient_matrix_UB_23      0.0549949000
_diffrn_orient_matrix_UB_31      -0.0531554000
_diffrn_orient_matrix_UB_32      0.0769718000
_diffrn_orient_matrix_UB_33      -0.0994187000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9899
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.461
_diffrn_reflns_theta_min         4.572
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.686
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91167
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_preparation       'diffusion of MeOH in CHCl3'
_exptl_crystal_recrystallization_method 'diffusion of MeOH in CHCl3'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.175
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         3167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0585P)^2^+0.2802P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2939
_reflns_number_total             3167
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01752g2.cif
_cod_data_source_block           exp_1123_a
_cod_depositor_comments
'Adding full bibliography for 7707781--7707784.cif.'
_cod_original_cell_volume        1509.27(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7707783
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C19 O1 N1 H11'
_cell_oxdiff_angle_alpha         90.033(3)
_cell_oxdiff_angle_beta          109.074(3)
_cell_oxdiff_angle_gamma         89.987(3)
_cell_oxdiff_length_a            10.7415(4)
_cell_oxdiff_length_b            10.8420(4)
_cell_oxdiff_length_c            13.7125(5)
_cell_oxdiff_measurement_reflns_used 6556
_cell_oxdiff_volume              1509.27(9)
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.847
_reflns_odcompleteness_completeness 98.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.17
_olex2_refinement_description
;
;
_shelx_res_checksum              4479
_shelx_hkl_checksum              96836