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_7708301
_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         '2(C24 H30 Br4 N2 Ni O3 Si2)'
_chemical_formula_sum            'C48 H60 Br8 N4 Ni2 O6 Si4'
_chemical_formula_weight         1658.06
_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   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                90
_cell_angle_beta                 109.483(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4499(13)
_cell_length_b                   23.9712(14)
_cell_length_c                   17.9196(12)
_cell_measurement_reflns_used    5698
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      24.9660
_cell_measurement_theta_min      1.7290
_cell_volume                     6256.6(8)
_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      180.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -10.00  48.00   1.00  100.00    --   17.79 -99.00 120.00   58
  2  \w    -25.00  30.00   1.00  100.00    --   17.79 -99.00  60.00   55
  3  \w    -17.00  20.00   1.00  100.00    --   17.79 -99.00 -30.00   37
  4  \w    -25.00  46.00   1.00  100.00    --   17.79 -99.00 -60.00   71
  5  \w      2.00  47.00   1.00  100.00    --   17.79  57.00-150.00   45
;
_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      0.0095734000
_diffrn_orient_matrix_UB_12      -0.0119678000
_diffrn_orient_matrix_UB_13      -0.0325780000
_diffrn_orient_matrix_UB_21      0.0162635000
_diffrn_orient_matrix_UB_22      -0.0245336000
_diffrn_orient_matrix_UB_23      0.0224825000
_diffrn_orient_matrix_UB_31      -0.0448846000
_diffrn_orient_matrix_UB_32      -0.0114470000
_diffrn_orient_matrix_UB_33      -0.0140180000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.1490
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30414
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.833
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64862
_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 brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.760
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         11048
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.1203
_refine_ls_R_factor_gt           0.0514
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6054
_reflns_number_total             11048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01980e2.cif
_cod_data_source_block           md_4271_mada
_cod_database_code               7708301
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N2Br2Si2Ni1
_chemical_oxdiff_usercomment     DS-108
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.388
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17A-C16A \\sim C17A-C16X
 with sigma of 0.01
 C16A-C15A \\sim C16X-C15X
 with sigma of 0.01
 Si2A-C15A \\sim Si2A-C15X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(C15A) = Uiso(C15X) = Uiso(C16X) = Uiso(C16A)
4. Others
 Fixed Sof: H17C(0.5) H17D(0.5) H17A(0.5) H17B(0.5) C16A(0.5) H16A(0.5)
 H16B(0.5) C16X(0.5) H16C(0.5) H16D(0.5) C15A(0.5) H15A(0.5) H15B(0.5)
 C15X(0.5) H15C(0.5) H15D(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C17A(H17C,H17D), C17A(H17A,
 H17B), C16A(H16A,H16B), C16X(H16C,H16D), C15A(H15A,H15B), C15X(H15C,H15D),
 C8B(H8BA,H8BB), C9B(H9BA,H9BB), C10B(H10C,H10D), C15B(H15E,H15F), C16B(H16E,
 H16F), C17B(H17E,H17F)
5.b Aromatic/amide H refined with riding coordinates:
 C18A(H18A), C3A(H3A), C5A(H5A), C7A(H7A), C20A(H20A), C22A(H22A), C3B(H3B),
 C5B(H5B), C7B(H7B), C18B(H18B), C20B(H20B), C22B(H22B)
5.c Idealised Me refined as rotating group:
 C11A(H11A,H11B,H11C), C12A(H12A,H12B,H12C), C13A(H13A,H13B,H13C), C14A(H14A,
 H14B,H14C), C11B(H11D,H11E,H11F), C12B(H12D,H12E,H12F), C13B(H13D,H13E,H13F),
 C14B(H14D,H14E,H14F)
;
_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 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.754