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_7708305
_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         'C24 H34 Cu N2 O5 Si2'
_chemical_formula_sum            'C24 H34 Cu N2 O5 Si2'
_chemical_formula_weight         550.25
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-07-30
_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                 96.812(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9833(18)
_cell_length_b                   14.3565(11)
_cell_length_c                   26.913(2)
_cell_measurement_reflns_used    2938
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.1850
_cell_measurement_theta_min      1.6330
_cell_volume                     5748.3(9)
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0797
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -18.00  25.00   1.00  100.00    --  -20.27 -99.00 150.00   43
  2  \w    -44.00  52.00   1.00  100.00    --  -20.27  77.00  60.00   96
  3  \w     65.00  91.00   1.00  100.00    --   22.30  57.00   0.00   26
  4  \w    -48.00  46.00   1.00  100.00    --   22.30 -57.00-150.00   94
;
_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      -0.0424808000
_diffrn_orient_matrix_UB_12      -0.0034693000
_diffrn_orient_matrix_UB_13      0.0090170000
_diffrn_orient_matrix_UB_21      -0.0064058000
_diffrn_orient_matrix_UB_22      0.0486791000
_diffrn_orient_matrix_UB_23      -0.0033837000
_diffrn_orient_matrix_UB_31      -0.0206674000
_diffrn_orient_matrix_UB_32      -0.0078865000
_diffrn_orient_matrix_UB_33      -0.0247165000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_unetI/netI     0.2586
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21655
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.610
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68391
_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    1.272
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         10114
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.823
_refine_ls_R_factor_all          0.2303
_refine_ls_R_factor_gt           0.0656
_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          0.0774
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3345
_reflns_number_total             10114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01980e2.cif
_cod_data_source_block           shi_4158_mada
_cod_depositor_comments
;

2024-09-23
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C48 H68 Cu2 N4 O10 Si4'
_cod_original_formula_weight         1100.50
_cod_original_formula_moiety         '2(C24 H34 Cu N2 O5 Si2)'
_cod_original_formula_units_Z            4
_cod_database_code               7708305
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N2O5Si1Cl2Mn1
_chemical_oxdiff_usercomment     DS36
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.880
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.114) H5A(0.201) H3A(0.103) H4A(0.128) H5AA(0.107)
 H7A(0.081) H8AA(0.098) H8AB(0.098) H9AA(0.087) H9AB(0.087) H10A(0.096)
 H10B(0.096) H11A(0.251) H11B(0.251) H11C(0.251) H12A(0.215) H12B(0.215)
 H12C(0.215) H13A(0.199) H13B(0.199) H13C(0.199) H14A(0.209) H14B(0.209)
 H14C(0.209) H15A(0.111) H15B(0.111) H16A(0.103) H16B(0.103) H17A(0.082)
 H17B(0.082) H18A(0.084) H20A(0.137) H21A(0.166) H22A(0.156) H2B(0.176)
 H5B(0.164) H3B(0.123) H4B(0.147) H5BA(0.137) H7B(0.093) H8BA(0.092)
 H8BB(0.092) H9BA(0.106) H9BB(0.106) H10C(0.108) H10D(0.108) H11D(0.201)
 H11E(0.201) H11F(0.201) H12D(0.152) H12E(0.152) H12F(0.152) H13D(0.161)
 H13E(0.161) H13F(0.161) H14D(0.158) H14E(0.158) H14F(0.158) H15C(0.109)
 H15D(0.109) H16C(0.098) H16D(0.098) H17C(0.095) H17D(0.095) H18B(0.09)
 H20B(0.102) H21B(0.126) H22B(0.118)
 Fixed X: H2A(0.367937) H5A(0.087544) H3A(0.27018) H4A(0.131854)
 H5AA(0.062677) H7A(0.061539) H8AA(0.030372) H8AB(0.069161) H9AA(0.190555)
 H9AB(0.098301) H10A(0.188066) H10B(0.097777) H11A(0.193516) H11B(0.102826)
 H11C(0.139956) H12A(0.256459) H12B(0.187469) H12C(0.288929) H13A(0.478652)
 H13B(0.530572) H13C(0.435722) H14A(0.434634) H14B(0.524924) H14C(0.444264)
 H15A(0.410602) H15B(0.508624) H16A(0.370362) H16B(0.471805) H17A(0.503877)
 H17B(0.439687) H18A(0.461511) H20A(0.444321) H21A(0.356806) H22A(0.202488)
 H2B(0.089261) H5B(0.497773) H3B(-0.102414) H4B(-0.123537) H5BA(-0.016244)
 H7B(0.125859) H8BA(0.245668) H8BB(0.334717) H9BA(0.302123) H9BB(0.318046)
 H10C(0.143972) H10D(0.169593) H11D(0.032807) H11E(0.075927) H11F(0.074717)
 H12D(0.273107) H12E(0.275507) H12F(0.336397) H13D(0.099737) H13E(0.124847)
 H13F(0.073137) H14D(0.363967) H14E(0.314377) H14F(0.286207) H15C(0.325052)
 H15D(0.301994) H16C(0.185222) H16D(0.168447) H17C(0.291715) H17D(0.216151)
 H18B(0.424261) H20B(0.575685) H21B(0.700334) H22B(0.6867)
 Fixed Y: H2A(0.476415) H5A(0.716499) H3A(0.326506) H4A(0.262851)
 H5AA(0.288078) H7A(0.356472) H8AA(0.406083) H8AB(0.503791) H9AA(0.428654)
 H9AB(0.405512) H10A(0.282885) H10B(0.259797) H11A(0.248846) H11B(0.227606)
 H11C(0.329736) H12A(0.106227) H12B(0.083627) H12C(0.100227) H13A(0.162772)
 H13B(0.215442) H13C(0.172382) H14A(0.406621) H14B(0.353771) H14C(0.301381)
 H15A(0.463851) H15B(0.425983) H16A(0.36978) H16B(0.343681) H17A(0.502355)
 H17B(0.456911) H18A(0.633381) H20A(0.783251) H21A(0.89714) H22A(0.875195)
 H2B(0.658577) H5B(0.497367) H3B(0.581163) H4B(0.495448) H5BA(0.492875)
 H7B(0.541463) H8BA(0.562171) H8BB(0.581849) H9BA(0.74371) H9BB(0.701737)
 H10C(0.727641) H10D(0.706536) H11D(0.873851) H11E(0.875831) H11F(0.966331)
 H12D(0.96629) H12E(0.86483) H12F(0.89135) H13D(1.09311) H13E(1.08848)
 H13F(1.0056) H14D(1.052819) H14E(1.132159) H14F(1.108789) H15C(0.898843)
 H15D(0.984865) H16C(0.834067) H16D(0.918009) H17C(0.86909) H17D(0.792909)
 H18B(0.823347) H20B(0.790081) H21B(0.70983) H22B(0.586966)
 Fixed Z: H2A(0.675477) H5A(0.850623) H3A(0.594876) H4A(0.603145)
 H5AA(0.673844) H7A(0.753394) H8AA(0.821388) H8AB(0.838957) H9AA(0.88685)
 H9AB(0.905668) H10A(0.847128) H10B(0.868389) H11A(1.016707) H11B(0.983327)
 H11C(0.987577) H12A(0.893024) H12B(0.930814) H12C(0.950514) H13A(0.958107)
 H13B(0.919347) H13C(0.902317) H14A(1.017596) H14B(1.013166) H14C(1.032816)
 H15A(0.910149) H15B(0.911846) H16A(0.84023) H16B(0.840788) H17A(0.824697)
 H17B(0.780901) H18A(0.854887) H20A(0.88497) H21A(0.914219) H22A(0.912731)
 H2B(0.787244) H5B(0.659643) H3B(0.73707) H4B(0.664082) H5BA(0.611745)
 H7B(0.590231) H8BA(0.55781) H8BB(0.593098) H9BA(0.588197) H9BB(0.53631)
 H10C(0.561905) H10D(0.508292) H11D(0.508172) H11E(0.457882) H11F(0.490382)
 H12D(0.480041) H12E(0.458701) H12F(0.508101) H13D(0.602263) H13E(0.660423)
 H13F(0.632103) H14D(0.601894) H14E(0.627784) H14F(0.571184) H15C(0.670876)
 H15D(0.70258) H16C(0.682231) H16D(0.717067) H17C(0.77454) H17D(0.767562)
 H18B(0.769954) H20B(0.786299) H21B(0.768617) H22B(0.713676)
;
_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 1.224
_oxdiff_exptl_absorpt_empirical_full_min 0.701