Nonconjugated Fluorescent Molecular Cages of Trinuclear Fluoroborate Complexes with Salicylaldehyde-Based Schiff Base Ligands.
Zhang, Xiaohong; Shi, Jun; Song, Jintong; Wang, Man; Xu, Xuemei; Qu, Lang; Zhou, Xiangge; Xiang, Haifeng; ACS omega 3 (2018) 8992–9002; doi:10.1021/acsomega.8b01504

data_4515942
_publ_section_title
;
 Nonconjugated Fluorescent Molecular Cages of Trinuclear Fluoroborate
 Complexes with Salicylaldehyde-Based Schiff Base Ligands.
;
_journal_issue                   8
_journal_name_full               'ACS omega'
_journal_page_first              8992
_journal_page_last               9002
_journal_paper_doi               10.1021/acsomega.8b01504
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C27 H21 B3 Cl6 F6 N4 O3'
_chemical_formula_sum            'C27 H21 B3 Cl6 F6 N4 O3'
_chemical_formula_weight         808.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-09-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.793(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.8016(4)
_cell_length_b                   12.2438(4)
_cell_length_c                   18.4551(5)
_cell_measurement_reflns_used    5180
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.3860
_cell_measurement_theta_min      3.2820
_cell_volume                     3295.84(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0874
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -46.00   -2.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -57.0000 -120.0000 44

  2 omega  -19.00   19.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669  -99.0000  -60.0000 38

  3 omega  -71.00  -36.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669 -178.0000  -90.0000 35

  4 omega   -2.00   45.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       16.6856   38.0000 -150.0000 47

  5 omega  -27.00   53.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -14.9669   77.0000 -150.0000 80
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0135490000
_diffrn_orient_matrix_UB_12      -0.0253271000
_diffrn_orient_matrix_UB_13      -0.0310136000
_diffrn_orient_matrix_UB_21      -0.0003433000
_diffrn_orient_matrix_UB_22      -0.0516365000
_diffrn_orient_matrix_UB_23      0.0173777000
_diffrn_orient_matrix_UB_31      -0.0467030000
_diffrn_orient_matrix_UB_32      -0.0069616000
_diffrn_orient_matrix_UB_33      -0.0160407000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0362
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16548
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         2.945
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.594
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.713
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         6726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0569
_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^)+(0.0478P)^2^+3.4320P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1421
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4898
_reflns_number_total             6726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b01504_si_004.cif
_cod_data_source_block           170921_s5_zxh
_cod_database_code               4515942
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         c12h12n2o3f2cl2
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.797
_reflns_odcompleteness_completeness 99.79
_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
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C11(H11A,H11B), C19(H19A,H19B),
 C20(H20A,H20B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C7(H7), C12(H12), C14(H14), C16(H16), C21(H21), C23(H23),
 C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'