Photo-induced crystallization with emission enhancement (PICEE)
Chen, Kongqi; Zhang, Rongyuan; Li, Ganggang; Li, Baoxi; Ma, Yao; Sun, Ming; Wang, Zhiming; Tang, Ben Zhong; Materials Horizons 7 (2020) 3005–3010; doi:10.1039/D0MH01200A

data_1558982
_publ_section_title
;
 Photo-induced crystallization with emission enhancement (PICEE)
;
_journal_issue                   11
_journal_name_full               'Materials Horizons'
_journal_page_first              3005
_journal_page_last               3010
_journal_paper_doi               10.1039/D0MH01200A
_journal_volume                  7
_journal_year                    2020
_chemical_formula_moiety
'4.02(C63.5 H55.5 N2 O2), 8(B F4), 1.5(C H2 Cl2), 2(H2 O)'
_chemical_formula_sum            'C256.5 H230 B8 Cl3 F32 N8 O10'
_chemical_formula_weight         4385.30
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-06
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-01-06 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                77.093(2)
_cell_angle_beta                 66.749(3)
_cell_angle_gamma                62.317(3)
_cell_formula_units_Z            1
_cell_length_a                   17.7648(7)
_cell_length_b                   18.0515(5)
_cell_length_c                   22.0097(7)
_cell_measurement_reflns_used    21198
_cell_measurement_temperature    119.99(13)
_cell_measurement_theta_max      73.1280
_cell_measurement_theta_min      2.7540
_cell_volume                     5735.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      119.99(13)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.932
_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     40.00  82.00   0.50    0.96    --    0.00  37.00   0.00   84
  2  \w    -14.00  50.00   0.50    0.96    --    0.00  72.00-180.00  128
  3  \w    -48.00   5.00   0.50    0.96    --    0.00 -57.00 -30.00  106
  4  \w    -89.00 -56.00   0.50    0.96    --    0.00 -72.00 120.00   66
  5  \w    -14.00  27.00   0.50    0.96    --    0.00  37.00   0.00   82
  6  \w     64.00  89.00   0.50    0.96    --    0.00  72.00-180.00   50
  7  \w    -53.00  13.00   0.50    0.96    --    0.00 -72.00 120.00  132
  8  \w    -88.00 -63.00   0.50    0.96    --    0.00 -57.00 -30.00   50
  9  \w    -74.00 -39.00   0.50    3.83    --  -98.80  72.00-180.00   70
 10  \w   -112.00 -11.00   0.50    3.83    --  -98.80  19.00 -90.00  202
 11  \w   -113.00 -83.00   0.50    3.83    --  -98.80  72.00-180.00   60
 12  \w   -113.00 -32.00   0.50    3.83    --  -98.80  72.00  60.00  162
 13  \w   -108.00 -42.00   0.50    3.83    --  -98.80  72.00-120.00  132
 14  \w    -92.00 -21.00   0.50    3.83    --  -98.80  72.00  90.00  142
 15  \w   -118.00 -85.00   0.50    3.83    --  -98.80 -72.00  60.00   66
 16  \w   -176.00-150.00   0.50    3.83    --  -98.80 -72.00  60.00   52
 17  \w   -112.00 -16.00   0.50    3.83    --  -98.80  72.00 120.00  192
 18  \w   -112.00 -28.00   0.50    3.83    --  -98.80  72.00 -60.00  168
 19  \w   -105.00 -10.00   0.50    3.83    --  -98.80  19.00   0.00  190
 20  \w    -85.00 -36.00   0.50    3.83    --  -98.80  57.00  30.00   98
 21  \w   -111.00 -84.00   0.50    3.83    --  -98.80  72.00   0.00   54
 22  \w   -112.00 -23.00   0.50    3.83    --  -98.80  72.00 -90.00  178
 23  \w   -110.00 -23.00   0.50    3.83    --  -98.80  72.00  30.00  174
 24  \w   -102.00 -60.00   0.50    3.83    --  -98.80  72.00 -30.00   84
 25  \w    -86.00 -35.00   0.50    3.83    --  -98.80  72.00 150.00  102
 26  \w    -93.00 -67.00   0.50    3.83    --  -98.80  72.00-150.00   52
 27  \w   -185.00 -11.00   0.50    3.83    --  -98.80   0.00 -60.00  348
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0913628000
_diffrn_orient_matrix_UB_12      0.0368465000
_diffrn_orient_matrix_UB_13      -0.0110866000
_diffrn_orient_matrix_UB_21      -0.0480702000
_diffrn_orient_matrix_UB_22      -0.0058382000
_diffrn_orient_matrix_UB_23      0.0752660000
_diffrn_orient_matrix_UB_31      -0.0127279000
_diffrn_orient_matrix_UB_32      0.0889874000
_diffrn_orient_matrix_UB_33      0.0054648000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            60619
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.928
_diffrn_reflns_theta_min         2.768
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_description       block
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.888
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1549
_refine_ls_number_reflns         21681
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1507
_refine_ls_R_factor_gt           0.1298
_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^)+(0.3200P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3850
_refine_ls_wR_factor_ref         0.4156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16249
_reflns_number_total             21681
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0mh01200a2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 1558982.cif.'
_cod_original_formula_sum        'C256.50 H230 B8 Cl3 F32 N8 O10'
_cod_database_code               1558982
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.811
_reflns_odcompleteness_completeness 98.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H,H) groups
2. Restrained distances
 Cl2-C1A = Cl3-C1A
 1.771 with sigma of 0.01
 Cl2-Cl3
 2.916 with sigma of 0.03
 Cl1-C1B = Cl4-C1B
 1.771 with sigma of 0.01
 Cl1-Cl4
 2.916 with sigma of 0.03
 B1-F1 \\sim B1-F2 \\sim B1-F3 \\sim B1-F4
 with sigma of 0.02
 F1-F2 \\sim F2-F3 \\sim F3-F4 \\sim F4-F1 \\sim F2-F4 \\sim F1-F3
 with sigma of 0.04
 B2-F5 \\sim B2-F6 \\sim B2-F7 \\sim B2-F8
 with sigma of 0.02
 F5-F6 \\sim F6-F7 \\sim F7-F8 \\sim F8-F5 \\sim F6-F8 \\sim F5-F7
 with sigma of 0.04
 B3-F9 \\sim B3-F10 \\sim B3-F11 \\sim B3-F12
 with sigma of 0.02
 F9-F10 \\sim F10-F11 \\sim F11-F12 \\sim F12-F9 \\sim F10-F12 \\sim F9-F11
 with sigma of 0.04
 B4-F13 \\sim B4-F14 \\sim B4-F15 \\sim B4-F16
 with sigma of 0.02
 F13-F14 \\sim F14-F15 \\sim F15-F16 \\sim F16-F13 \\sim F14-F16 \\sim F13-F15
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
B1 \\sim F1 \\sim F2 \\sim F3 \\sim F4: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
B2 \\sim F5 \\sim F6 \\sim F7 \\sim F8: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
B3 \\sim F9 \\sim F10 \\sim F11 \\sim F12: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
B4 \\sim F13 \\sim F14 \\sim F15 \\sim F16: within 1.7A with sigma of 0.02 and
sigma for terminal atoms of 0.04
Cl2 \\sim Cl3 \\sim C1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Cl1 \\sim Cl4 \\sim C1B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C50) = Uanis(C124)
Uanis(Cl2) = Uanis(C1A)
Uanis(C70) = Uanis(C95)
4. Rigid body (RIGU) restrains
 B1, F1, F2, F3, F4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F5, F6, F7, F8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B3, F9, F10, F11, F12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B4, F13, F14, F15, F16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl2, Cl3, C1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1, Cl4, C1B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H50(0.5) H50A(0.5) H89(0.5) H89A(0.5) C95(0.5) H95(0.5) C115(0.5)
 H115(0.5) C116(0.5) H116(0.5) C117(0.5) C118(0.5) H118(0.5) C119(0.5)
 H119(0.5) C120(0.5) H120(0.5) C121(0.5) N4(0.5) C122(0.5) H122(0.5) C123(0.5)
 C124(0.5) C125(0.5) C126(0.5) H126(0.5) C127(0.5) H127(0.5) C128(0.5)
 C129(0.5) H129(0.5) C130(0.5) H130(0.5) C131(0.5) H131(0.5) C132(0.5)
 C133(0.5) N5(0.5) C134(0.5) H134(0.5) C135(0.5) C136(0.5) C137(0.5) H13A(0.5)
 H13B(0.5) C138(0.5) H13C(0.5) H13D(0.5) C139(0.5) H13E(0.5) H13F(0.5)
 C140(0.5) H14A(0.5) H14B(0.5) C141(0.5) H14C(0.5) H14D(0.5) H14E(0.5)
 C142(0.5) H14F(0.5) H14G(0.5) H14H(0.5) Cl2(0.5) Cl3(0.5) C1A(0.5) H1AA(0.5)
 H1AB(0.5) Cl1(0.25) Cl4(0.25) C1B(0.25) H1BA(0.25) H1BB(0.25)
6.a Free rotating group:
 O0AA(H0AA,H0AB)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C91(H91A,H91B), C104(H10D,H10E), C105(H10I,H10J), C108(H10K,
 H10L), C114(H11G,H11H), C137(H13A,H13B), C138(H13C,H13D), C139(H13E,H13F),
 C140(H14A,H14B), C1A(H1AA,H1AB), C1B(H1BA,H1BB)
6.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C12(H12), C14(H14), C20(H20), C23(H23),
 C31(H31), C34(H34), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C50(H50A), C51(H51), C52(H52), C53(H53),
 C54(H54), C56(H56), C57(H57), C59(H59), C61(H61), C63(H63), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68), C69(H69), C70(H70), C71(H71), C72(H72),
 C73(H73), C74(H74), C76(H76), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82),
  C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89),
 C89(H89A), C90(H90), C92(H92), C93(H93), C95(H95), C96(H96), C97(H97),
 C98(H98), C99(H99), C100(H100), C102(H102), C106(H106), C107(H107), C109(H109),
  C112(H112), C115(H115), C116(H116), C118(H118), C119(H119), C120(H120),
 C122(H122), C126(H126), C127(H127), C129(H129), C130(H130), C131(H131),
 C134(H134)
6.d Fitted hexagon refined as free rotating group:
 C115(C116,C117,C118,C119,C120), C121(N4,C122,C123,C124,C125), C126(C127,C128,
 C129,C130,C131), C132(C133,N5,C134,C135,C136)
6.e Idealised Me refined as rotating group:
 C77(H77A,H77B,H77C), C94(H94A,H94B,H94C), C101(H10A,H10B,H10C), C103(H10F,
 H10G,H10H), C110(H11A,H11B,H11C), C111(H11I,H11J,H11K), C113(H11D,H11E,H11F),
 C141(H14C,H14D,H14E), C142(H14F,H14G,H14H)
;
_shelx_res_checksum              57237
_platon_squeeze_void_probe_radius 1.20
_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 1.437
_oxdiff_exptl_absorpt_empirical_full_min 0.611