Dual crystalline-amorphous salen-metal complexes behave like nematic droplets with AIEgens vistas.
Damoc, Madalin; Stoica, Alexandru-Constantin; Dascalu, Mihaela; Asandulesa, Mihai; Shova, Sergiu; Cazacu, Maria; Dalton transactions (Cambridge, England : 2003)  (2021) –; doi:10.1039/d1dt01980e

data_7708303
_publ_section_title
;
 Dual crystalline-amorphous salen-metal complexes behave like nematic
 droplets with AIEgens vistas.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/d1dt01980e
_journal_year                    2021
_chemical_formula_moiety         '3(C24 H30 Cl4 N2 O3 Si2 Zn), C H2 Cl2'
_chemical_formula_sum            'C73 H92 Cl14 N6 O9 Si6 Zn3'
_chemical_formula_weight         2058.47
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-02-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-01 deposited with the CCDC.	2021-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                99.587(3)
_cell_angle_beta                 104.598(4)
_cell_angle_gamma                109.175(4)
_cell_formula_units_Z            2
_cell_length_a                   15.6914(9)
_cell_length_b                   17.4652(7)
_cell_length_c                   19.6006(8)
_cell_measurement_reflns_used    6281
_cell_measurement_temperature    180.05(10)
_cell_measurement_theta_max      24.6710
_cell_measurement_theta_min      1.5310
_cell_volume                     4723.6(4)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -28.00  46.00   1.00   30.00    --  -15.76  57.00  30.00   74
  2  \w      2.00  79.00   1.00   30.00    --   17.94  57.00 120.00   77
  3  \w      6.00  78.00   1.00   30.00    --   17.94  57.00 -90.00   72
  4  \w     16.00  83.00   1.00   30.00    --   17.94  57.00-180.00   67
  5  \w    -23.00  23.00   1.00   30.00    --  -15.76 -99.00   0.00   46
  6  \w    -32.00  29.00   1.00   30.00    --  -15.76  57.00 -30.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0485654000
_diffrn_orient_matrix_UB_12      -0.0092534000
_diffrn_orient_matrix_UB_13      -0.0192567000
_diffrn_orient_matrix_UB_21      -0.0050116000
_diffrn_orient_matrix_UB_22      -0.0404048000
_diffrn_orient_matrix_UB_23      -0.0188917000
_diffrn_orient_matrix_UB_31      -0.0136156000
_diffrn_orient_matrix_UB_32      -0.0167111000
_diffrn_orient_matrix_UB_33      0.0279836000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_av_unetI/netI     0.1070
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            35173
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.280
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76709
_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            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         16648
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1254
_refine_ls_R_factor_gt           0.0823
_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^)+(0.0490P)^2^+12.2125P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11272
_reflns_number_total             16648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01980e2.cif
_cod_data_source_block           shi_4176_mada
_cod_database_code               7708303
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N2O4Cl2Si2Zn1
_chemical_oxdiff_usercomment     DS_39
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.628
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Restrained distances
 Cl2-C1X \\sim Cl2X-C1X
 with sigma of 0.01
 Cl2X-C1X \\sim Cl2-C1
 with sigma of 0.01
 Cl1-C1X \\sim Cl1-C1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl2X) = Uanis(Cl2)
Uanis(C1X) = Uanis(C1)
4. Others
 Sof(Cl2X)=Sof(C1X)=Sof(H7DA)=Sof(H8DA)=1-FVAR(1)
 Sof(Cl2)=Sof(C1)=Sof(H5DA)=Sof(H6DA)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C8A(HC,HD), C9A(HE,HF), C10A(HG,HH), C15A(HU,HV), C16A(HW,HX), C17A(HY,HZ),
 C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10A,H10B), C15B(H15A,H15B), C16B(H16A,
 H16B), C17B(H17A,H17B), C8C(H6AA,H7AA), C9C(H8AA,H9AA), C10C(H0BA,H1BA),
 C15C(H6CA,H7CA), C16C(H8CA,H9CA), C17C(H0DA,H1DA), C1(H5DA,H6DA), C1X(H7DA,
 H8DA)
5.b Aromatic/amide H refined with riding coordinates:
 C3A(H), C5A(HA), C7A(HB), C18A(H0AA), C20A(H1AA), C22A(H2AA), C3B(H3B),
 C5B(H5B), C7B(H7B), C18B(H18B), C20B(H20B), C22B(H22B), C3C(H3AA), C5C(H4AA),
 C7C(H5AA), C18C(H2DA), C20C(H3DA), C22C(H4DA)
5.c Idealised Me refined as rotating group:
 C11A(HI,HJ,HK), C12A(HL,HM,HN), C13A(HO,HP,HQ), C14A(HR,HS,HT), C11B(H11A,
 H11B,H11C), C12B(H12A,H12B,H12C), C13B(H13A,H13B,H13C), C14B(H14A,H14B,H14C),
 C11C(H2BA,H3BA,H4BA), C12C(H5BA,H6BA,H7BA), C13C(H0CA,H1CA,H2CA), C14C(H3CA,
 H4CA,H5CA)
;
_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 1.207
_oxdiff_exptl_absorpt_empirical_full_min 0.800