Supramolecular Solid-State Microlaser Constructed from Pillar[5]arene-Based Host-Guest Complex Microcrystals.
Hua, Bin; Zhou, Wei; Yang, Zhaoliang; Zhang, Zhihua; Shao, Li; Zhu, Haiming; Huang, Feihe; Journal of the American Chemical Society 140 (2018) 15651–15654; doi:10.1021/jacs.8b11156

data_4133561
_publ_section_title
;
 Supramolecular Solid-State Microlaser Constructed from
 Pillar[5]arene-Based Host-Guest Complex Microcrystals.
;
_journal_issue                   46
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15651
_journal_page_last               15654
_journal_paper_doi               10.1021/jacs.8b11156
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'I, 2(C55 H60 Br10 O10), C16 H19 N2'
_chemical_formula_sum            'C126 H139 Br20 I N2 O20'
_chemical_formula_weight         3726.28
_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     dual
_audit_creation_date             2018-09-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                82.203(4)
_cell_angle_beta                 81.506(4)
_cell_angle_gamma                76.519(4)
_cell_formula_units_Z            1
_cell_length_a                   12.3928(6)
_cell_length_b                   15.6251(7)
_cell_length_c                   18.2747(9)
_cell_measurement_reflns_used    4933
_cell_measurement_temperature    127.6
_cell_measurement_theta_max      29.2827
_cell_measurement_theta_min      3.0266
_cell_volume                     3384.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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_temperature      127.6
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -86.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683  -77.0000 -150.0000 93

  2 omega  -38.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683   77.0000   90.0000 88

  3 omega  -87.00   12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.4683  -67.0000  -36.0000 99
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0229707000
_diffrn_orient_matrix_UB_12      -0.0310909000
_diffrn_orient_matrix_UB_13      0.0258812000
_diffrn_orient_matrix_UB_21      0.0403792000
_diffrn_orient_matrix_UB_22      -0.0350712000
_diffrn_orient_matrix_UB_23      -0.0154787000
_diffrn_orient_matrix_UB_31      0.0368371000
_diffrn_orient_matrix_UB_32      0.0026263000
_diffrn_orient_matrix_UB_33      0.0254537000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0910
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22056
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         3.033
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.203
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       block
_exptl_crystal_F_000             1822
_refine_diff_density_max         2.300
_refine_diff_density_min         -1.558
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         12814
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1271
_refine_ls_R_factor_gt           0.0757
_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^)+(0.0741P)^2^+22.8023P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1686
_refine_ls_wR_factor_ref         0.2031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8157
_reflns_number_total             12814
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b11156_si_002.cif
_cod_data_source_block           170608_hb_1_4th
_cod_database_code               4133561
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'c10 h10 n2 o8 br1'
_reflns_odcompleteness_completeness 99.71
_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
 C40-Br7A = C55-Br = C35-Br6A
 2 with sigma of 0.02
 C63-C60
 1.4 with sigma of 0.02
 C63-C64
 1.4 with sigma of 0.02
 C64-C65
 1.4 with sigma of 0.02
 C60-C64 = C63-C65
 2.4 with sigma of 0.02
 C55-C54
 1.5 with sigma of 0.02
 C68-C64 \\sim C64-C67
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C73) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C58)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(N1) \\sim Ueq,
Uanis(C62) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(C68) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(C66) \\sim Ueq,
Uanis(C74) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C72)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C54) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Br, Br10, O2, C54, C55
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C65, C59, C60, C58, C61, C63, C64, N1, C62, C56, C68, C67, C66, C73, C74, N2,
 C71, C72
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2, C54, C55, Br, Br10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(Br4A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(Br4)=Sof(H24A)=Sof(H24B)=FVAR(1)
 Sof(Br7A)=Sof(H40C)=Sof(H40D)=1-FVAR(2)
 Sof(Br7)=Sof(H40A)=Sof(H40B)=FVAR(2)
 Sof(Br6A)=Sof(H35C)=Sof(H35D)=1-FVAR(3)
 Sof(Br6)=Sof(H35A)=Sof(H35B)=FVAR(3)
 Sof(Br)=Sof(H55C)=Sof(H55D)=1-FVAR(4)
 Sof(Br10)=Sof(H55A)=Sof(H55B)=FVAR(4)
 Sof(H46C)=Sof(H46D)=Sof(Br8A)=1-FVAR(5)
 Sof(Br8)=Sof(H46A)=Sof(H46B)=FVAR(5)
 Fixed Sof: I1(0.5) C59(0.5) H59(0.5) C60(0.5) C61(0.5) H61(0.5) C62(0.5)
 H62(0.5) N1(0.5) C58(0.5) H58(0.5) C74(0.5) C66(0.5) H66(0.5) C68(0.5)
 H68(0.5) C65(0.5) C67(0.5) H67(0.5) C73(0.5) H73(0.5) C63(0.5) H63(0.5)
 N2(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) C56(0.5) H56A(0.5) H56B(0.5)
 H56C(0.5) C72(0.5) H72A(0.5) H72B(0.5) H72C(0.5) C64(0.5) H64(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B),
 C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B), C23(H23A,H23B), C24(H24A,H24B),
  C24(H24C,H24D), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C34(H34A,
 H34B), C35(H35A,H35B), C35(H35C,H35D), C39(H39A,H39B), C40(H40A,H40B),
 C40(H40C,H40D), C42(H42A,H42B), C45(H45A,H45B), C46(H46A,H46B), C46(H46C,H46D),
  C50(H50A,H50B), C51(H51A,H51B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C55(H55C,H55D)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C14(H14), C19(H19), C25(H25), C30(H30), C36(H36), C41(H41),
 C47(H47), C52(H52), C59(H59), C61(H61), C62(H62), C58(H58), C66(H66), C68(H68),
  C67(H67), C73(H73), C63(H63), C64(H64)
6.c Fitted hexagon refined as free rotating group:
 C59(C60,C61,C62,N1,C58), C74(C66,C68,C65,C67,C73)
6.d Idealised Me refined as rotating group:
 C71(H71A,H71B,H71C), C56(H56A,H56B,H56C), C72(H72A,H72B,H72C)
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_shelx_res_checksum              76025
_shelx_hkl_checksum              45046
_olex2_submission_special_instructions 'No special instructions were received'