Rotors tailoring molecular stacking for constructing multi-stimuli-responsive luminescent materials.
Liu, Zheng-Fei; Zeng, Lan; Niu, Li-Ya; Yang, Qing-Zheng; Chemical communications (Cambridge, England) 59 (2023) 2453–2456; doi:10.1039/d2cc06847h

data_7131270
_publ_section_title
;
 Rotors tailoring molecular stacking for constructing
 multi-stimuli-responsive luminescent materials.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2453
_journal_page_last               2456
_journal_paper_doi               10.1039/d2cc06847h
_journal_volume                  59
_journal_year                    2023
_chemical_formula_moiety         'C17 H15 B F2 N2 O2 S'
_chemical_formula_sum            'C17 H15 B F2 N2 O2 S'
_chemical_formula_weight         360.208
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2022-12-21
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2022.12.14 svn.re48b8309 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-01-07 deposited with the CCDC.	2023-01-31 downloaded from the CCDC.
;
_cell_angle_alpha                109.969(2)
_cell_angle_beta                 99.326(2)
_cell_angle_gamma                104.781(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4059(2)
_cell_length_b                   9.7970(2)
_cell_length_c                   11.4192(2)
_cell_measurement_reflns_used    7536
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9500
_cell_measurement_theta_min      4.2790
_cell_volume                     821.86(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.9953
_diffrn_measured_fraction_theta_max 0.9474
_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    -21.00  36.00   0.50    0.05    --   46.95 -29.00  -2.00  114
  2  \w    -16.00  56.00   0.50    0.05    --   46.95 -57.00 -30.00  144
  3  \w     37.00 102.00   0.50    0.05    --  104.75 -94.00 -90.00  130
  4  \w     77.00 108.00   0.50    0.05    --  104.75 -94.00 -60.00   62
  5  \w     71.00 108.00   0.50    0.05    --  104.75 -77.00  60.00   74
  6  \w     62.00 117.00   0.50    0.05    --  104.75-125.00  60.00  110
  7  \w     38.00  70.00   0.50    0.05    --  104.75 -61.00 120.00   64
  8  \w     33.00  66.00   0.50    0.05    --  104.75 -61.00  90.00   66
  9  \w     35.00 108.00   0.50    0.05    --  104.75 -94.00  60.00  146
 10  \w     39.00  64.00   0.50    0.05    --  104.75 -94.00 -60.00   50
 11  \w     35.00  65.00   0.50    0.05    --  104.75 -61.00 -60.00   60
 12  \w     34.00  65.00   0.50    0.05    --  104.75 -61.00-180.00   62
 13  \w     43.00  74.00   0.50    0.05    --  104.75 -94.00-180.00   62
 14  \w     77.00 107.00   0.50    0.05    --  104.75 -94.00-180.00   60
 15  \w     92.00 172.00   0.50    0.05    --  104.75  45.00  30.00  160
 16  \w    139.00 168.00   0.50    0.05    --  104.75  61.00  90.00   58
 17  \w    129.00 178.00   0.50    0.05    --  104.75  29.00 158.00   98
 18  \w     97.00 123.00   0.50    0.05    --  104.75  61.00  90.00   52
 19  \w     92.00 175.00   0.50    0.05    --  104.75  15.00 120.00  166
 20  \w     57.00  95.00   0.50    0.05    --   46.95  29.00 158.00   76
 21  \w    -31.00   7.00   0.50    0.05    --  -46.95  29.00 158.00   76
 22  \w    -71.00 -34.00   0.50    0.05    -- -102.00 125.00  30.00   74
 23  \w    -69.00 -44.00   0.50    0.05    -- -102.00  61.00  30.00   50
 24  \w    -69.00 -40.00   0.50    0.05    -- -102.00  61.00   0.00   58
 25  \w    -40.00  -5.00   0.50    0.05    --  -46.95  37.00-120.00   70
 26  \w    -23.00   6.00   0.50    0.05    --  -46.95  57.00-180.00   58
 27  \w    -62.00 -27.00   0.50    0.05    --  -46.95  57.00-180.00   70
 28  \w    -63.00 -33.00   0.50    0.05    -- -102.00  61.00-120.00   60
 29  \w   -116.00 -51.00   0.50    0.05    -- -102.00 125.00-150.00  130
 30  \w   -117.00 -92.00   0.50    0.05    -- -102.00 125.00  30.00   50
 31  \w   -111.00 -82.00   0.50    0.05    -- -102.00 125.00 150.00   58
 32  \w    -71.00 -34.00   0.50    0.05    -- -102.00 125.00 150.00   74
 33  \w   -121.00 -74.00   0.50    0.05    --  -46.95 -29.00  -2.00   94
 34  \w    -23.00  17.00   0.50    0.05    --   46.95 -19.00-150.00   80
 35  \w    147.00 173.00   0.50    0.05    --  104.75  45.00-180.00   52
 36  \w   -169.00-108.00   0.50    0.05    -- -102.00 -29.00  -2.00  122
 37  \w   -171.00 -91.00   0.50    0.05    -- -102.00 -30.00 -90.00  160
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.9953
_diffrn_reflns_Laue_measured_fraction_max 0.9474
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8864
_diffrn_reflns_point_group_measured_fraction_full 0.9953
_diffrn_reflns_point_group_measured_fraction_max 0.9474
_diffrn_reflns_theta_full        67.6840
_diffrn_reflns_theta_max         76.54
_diffrn_reflns_theta_min         4.28
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56701
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark brown'
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             374.004
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.2353
_refine_diff_density_min         -0.2370
_refine_diff_density_rms         0.0344
_refine_ls_d_res_high            0.7927
_refine_ls_d_res_low             10.3213
_refine_ls_extinction_coef       0.0103
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0921
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    41
_refine_ls_number_parameters     348
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     187
_refine_ls_restrained_S_all      1.0589
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          -0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.1078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              11
_reflns_limit_k_min              -12
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3124
_reflns_number_total             3278
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2cc06847h2.cif
_cod_data_source_block           20210702b-snbfn
_cod_depositor_comments
'Adding full bibliography for 7131269--7131270.cif.'
_cod_database_code               7131270
_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
 S1-C00H \\sim S1a-C00H
 with sigma of 0.02
 S1-C00K \\sim S1a-C2
 with sigma of 0.02
 C10-C00H \\sim C10a-C00H
 with sigma of 0.02
 C10-C00I \\sim C10a-C1
 with sigma of 0.02
 S1-C00I \\sim S1a-C1
 with sigma of 0.04
 C00I-C00K \\sim C1-C2
 with sigma of 0.02
 C10-C00K \\sim C10a-C2
 with sigma of 0.04
 C00H-C00I \\sim C00H-C1
 with sigma of 0.04
 C00H-C00K \\sim C00H-C2
 with sigma of 0.04
 N8-C00C \\sim N8a-C00C
 with sigma of 0.02
 N8-C00M \\sim N8a-C00n
 with sigma of 0.02
 N8-C00O \\sim N8a-C5
 with sigma of 0.02
 C00C-C00L \\sim C00C-C4
 with sigma of 0.02
 C00J-H00J \\sim C3-H3
 with sigma of 0.02
 C00J-C00L \\sim C3-C4
 with sigma of 0.02
 C00J-C00M \\sim C3-C00n
 with sigma of 0.02
 C00L-H00L \\sim C4-H4
 with sigma of 0.02
 C00M-H00M \\sim C00n-H00o
 with sigma of 0.02
 C00O-C00P \\sim C5-C00q
 with sigma of 0.02
 N8-C00J \\sim N8a-C3
 with sigma of 0.04
 N8-H00M \\sim N8a-H00o
 with sigma of 0.04
 N8-C00P \\sim N8a-C00q
 with sigma of 0.04
 C00C-C00J \\sim C00C-C3
 with sigma of 0.04
 C00C-H00L \\sim C00C-H4
 with sigma of 0.04
 C00C-C00M \\sim C00C-C00n
 with sigma of 0.04
 C00C-C00O \\sim C00C-C5
 with sigma of 0.04
 C00J-H00L \\sim C3-H4
 with sigma of 0.04
 C00J-H00M \\sim C3-H00o
 with sigma of 0.04
 H00J-C00L \\sim H3-C4
 with sigma of 0.04
 H00J-C00M \\sim H3-C00n
 with sigma of 0.04
 C00L-C00M \\sim C4-C00n
 with sigma of 0.04
 C00M-C00O \\sim C00n-C5
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
S1 \\sim C10a: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.002 within 2A
S1a \\sim C10: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Uanis(C10) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 S1a, C10a, C2, C1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C5, C00q, N8a, C00n, C3, C4, C00C
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C00P, C00O, N8, C00C, C00L, C00M, C00J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1a)=Sof(C10a)=Sof(H10a)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=1-FVAR(1)
 Sof(S1)=Sof(C10)=Sof(H10)=Sof(C00I)=Sof(H00I)=Sof(C00K)=Sof(H00K)=FVAR(1)
 Sof(N8a)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C00n)=Sof(H00o)=Sof(C5)=Sof(H5a)=
 Sof(H5b)=Sof(C00q)=Sof(H00p)=Sof(H00q)=Sof(H00r)=1-FVAR(2)
 Sof(N8)=Sof(C00J)=Sof(H00J)=Sof(C00L)=Sof(H00L)=Sof(C00M)=Sof(H00M)=Sof(C00O)=
 Sof(H00a)=Sof(H00b)=Sof(C00P)=Sof(H00c)=Sof(H00h)=Sof(H00n)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C00O(H00a,H00b), C5(H5a,H5b)
6.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00I(H00I),
 C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C10a(H10a), C1(H1), C2(H2),
 C3(H3), C4(H4), C00n(H00o)
6.c Idealised Me refined as rotating group:
 C00P(H00c,H00h,H00n), C00q(H00p,H00q,H00r)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
 - for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 5.0
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Normal
   METHOD:         R2SCAN
   BASIS SET:      def2-TZVP
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2022-12-21_11-31-40
;
_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
;