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_7708304
_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 H30 Cl4 Co N2 O3 Si2, 1/3(C H2 Cl2)'
_chemical_formula_sum            'C24.3333 H30.66667 Cl4.66667 Co N2 O3 Si2'
_chemical_formula_weight         679.72
_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                99.440(4)
_cell_angle_beta                 104.592(4)
_cell_angle_gamma                109.205(5)
_cell_formula_units_Z            6
_cell_length_a                   15.6932(7)
_cell_length_b                   17.4257(10)
_cell_length_c                   19.5315(9)
_cell_measurement_reflns_used    7839
_cell_measurement_temperature    180.1(2)
_cell_measurement_theta_max      25.6330
_cell_measurement_theta_min      1.5240
_cell_volume                     4699.7(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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      180.1(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  23.00   1.00  100.00    --  -15.60 -99.00-120.00   41
  2  \w     65.00  90.00   1.00  100.00    --   17.79-178.00   0.00   25
  3  \w    -10.00  52.00   1.00  100.00    --   17.79 -99.00 150.00   62
  4  \w    -19.00   7.00   1.00  100.00    --  -15.60 -99.00  30.00   26
  5  \w    -22.00  56.00   1.00  100.00    --   17.79 -99.00  30.00   78
  6  \w    -20.00  87.00   1.00  100.00    --   17.79   0.00   0.00  107
  7  \w      2.00  84.00   1.00  100.00    --   17.79  38.00-120.00   82
;
_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      -0.0248448000
_diffrn_orient_matrix_UB_12      -0.0215476000
_diffrn_orient_matrix_UB_13      -0.0376812000
_diffrn_orient_matrix_UB_21      0.0132813000
_diffrn_orient_matrix_UB_22      -0.0343314000
_diffrn_orient_matrix_UB_23      0.0052262000
_diffrn_orient_matrix_UB_31      -0.0421177000
_diffrn_orient_matrix_UB_32      -0.0190052000
_diffrn_orient_matrix_UB_33      0.0084788000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0720
_diffrn_reflns_av_unetI/netI     0.1649
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37110
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83729
_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 orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       prism
_exptl_crystal_F_000             2094
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.570
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1012
_refine_ls_number_reflns         16537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.1127
_refine_ls_R_factor_gt           0.0515
_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          0.0659
_refine_ls_wR_factor_ref         0.0845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9380
_reflns_number_total             16537
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01980e2.cif
_cod_data_source_block           md_4270_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            'C73 H92 Cl14 Co3 N6 O9 Si6'
_cod_original_formula_weight         2039.15
_cod_original_formula_moiety         '3(C24 H30 Cl4 Co N2 O3 Si2), C H2 Cl2'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        4699.7(4)
_cod_database_code               7708304
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C30H30N2O4Cl2Si2Co1
_chemical_oxdiff_usercomment     C105
_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.622
_reflns_odcompleteness_completeness 99.69
_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.a Secondary CH2 refined with riding coordinates:
 C16A(HE,HF), C17A(HG,HH), C16B(HI,HJ), C17B(HM,HN), C9C(H9CA,H9CB), C8A(HO,
 HP), C8B(HR,HS), C17C(H17A,H17B), C15B(HV,HW), C9B(HY,HZ), C15A(H0AA,H1AA),
 C9A(H2AA,H3AA), C16C(H16A,H16B), C8C(H8CA,H8CB), C10C(H10A,H10B), C10A(H5AA,
 H6AA), C15C(H15A,H15B), C10B(H7AA,H8AA), C1(H5DA,H6DA)
2.b Aromatic/amide H refined with riding coordinates:
 C7A(H), C18A(HA), C3B(HB), C20C(H20C), C3A(HC), C7C(H7C), C5A(HD), C7B(HK),
 C22A(HL), C18C(H18C), C20A(HQ), C22C(H22C), C5C(H5C), C20B(HT), C18B(HU),
 C5B(HX), C3C(H3C), C22B(H4AA)
2.c Idealised Me refined as rotating group:
 C14B(H9AA,H0BA,H1BA), C14A(H2BA,H3BA,H4BA), C12A(H5BA,H6BA,H7BA), C13B(H8BA,
 H9BA,H0CA), C13A(H1CA,H2CA,H3CA), C14C(H14A,H14B,H14C), C11A(H4CA,H5CA,H6CA),
 C11B(H7CA,H0DA,H1DA), C11C(H11A,H11B,H11C), C12C(H12A,H12B,H12C), C13C(H13A,
 H13B,H13C), C12B(H2DA,H3DA,H4DA)
;
_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 1.204
_oxdiff_exptl_absorpt_empirical_full_min 0.795