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_7707781
_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         'C44 H28 N2 O3 Zn, C4 H8 O'
_chemical_formula_sum            'C48 H36 N2 O4 Zn'
_chemical_formula_weight         770.16
_chemical_name_systematic        'Zn salen phenyl bis[4]helicene'
_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
_audit_creation_date             2021-04-27
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2021-04-29 deposited with the CCDC.	2021-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.19(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1499(14)
_cell_length_b                   30.4057(15)
_cell_length_c                   17.238(3)
_cell_measurement_reflns_used    1139
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      63.6830
_cell_measurement_theta_min      5.3330
_cell_volume                     3654.2(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3980
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.963
_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    -38.00  26.00   0.50    7.28    --   41.11 -19.00  90.00  128
  2  \w    -15.00  82.00   0.50    7.28    --   41.11 -99.00   0.00  194
  3  \w     21.00 106.00   0.50   24.98    --  103.45 -94.00  30.00  170
  4  \w     42.00  71.00   0.50   24.98    --  103.45 -61.00  90.00   58
  5  \w     82.00 158.00   0.50   24.98    --  103.45 125.00  30.00  152
  6  \w     78.00 106.00   0.50   24.98    --  103.45  45.00-180.00   56
  7  \w     82.00 158.00   0.50   24.98    --  103.45  77.00  90.00  152
  8  \w    115.00 149.00   0.50   24.98    --  103.45  45.00-180.00   68
  9  \w     82.00 147.00   0.50   24.98    --  103.45  77.00-150.00  130
 10  \w     90.00 150.00   0.50   24.98    --  103.45  45.00 150.00  120
;
_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      -0.2103579000
_diffrn_orient_matrix_UB_12      -0.0051853000
_diffrn_orient_matrix_UB_13      -0.0771870000
_diffrn_orient_matrix_UB_21      0.0207544000
_diffrn_orient_matrix_UB_22      0.0404148000
_diffrn_orient_matrix_UB_23      -0.0481338000
_diffrn_orient_matrix_UB_31      0.0640870000
_diffrn_orient_matrix_UB_32      -0.0301297000
_diffrn_orient_matrix_UB_33      -0.0513877000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.1345
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13239
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.887
_diffrn_reflns_theta_min         3.331
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
'CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019) Numerical absorption correction based on gaussian integration over 			a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       needle
_exptl_crystal_F_000             1600
_exptl_crystal_preparation       'vapor diffusion of MeOH in THF'
_exptl_crystal_recrystallization_method 'vapor diffusion of MeOH in THF'
_exptl_crystal_size_max          0.247
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.888
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1700
_refine_ls_R_factor_gt           0.0933
_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^)+(0.0961P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2875
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3232
_reflns_number_total             6896
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01752g2.cif
_cod_data_source_block           exp_1177_a
_cod_depositor_comments
'Adding full bibliography for 7707781--7707784.cif.'
_cod_database_code               7707781
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C52N2O2Zn1C26
_chemical_oxdiff_usercomment     'Crystallized from CHCl3/MeOH'
_cell_oxdiff_angle_alpha         90.046(7)
_cell_oxdiff_angle_beta          121.168(14)
_cell_oxdiff_angle_gamma         89.971(9)
_cell_oxdiff_length_a            8.1514(13)
_cell_oxdiff_length_b            30.401(2)
_cell_oxdiff_length_c            17.234(2)
_cell_oxdiff_measurement_reflns_used 1140
_cell_oxdiff_volume              3654.2(7)
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.734
_diffrn_oxdiff_digest_frames
;
019b3d0cf3c67e568d9f6d5c6ad6853bee01280435b
;
_diffrn_oxdiff_digest_hkl
;
01da44ffbcda5557eb953f1dce434a51a0b40c
;
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O4-H4A = O4-H4B
 0.96 with sigma of 0.02
 H4A-H4B
 1.63 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C1 \\sim O1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4C,H4D)
4.b Aromatic/amide H refined with riding coordinates:
 C23(H23), C30(H30), C19(H19), C22(H22), C36(H36), C33(H33), C48(H48),
 C25(H25), C11(H11), C16(H16), C28(H28), C37(H37), C38(H38), C45(H45), C15(H15),
  C5(H5), C12(H12), C42(H42), C46(H46), C47(H47), C26(H26), C41(H41), C27(H27),
 C8(H8), C6(H6), C7(H7)
;
_shelx_res_checksum              19910
_shelx_hkl_checksum              9511