Temperature-dependent Interchromophoric Interaction in a Fluorescent Pyrene-based Metal‒organic Framework
Gladysiak, Andrzej; Nguyen, Tu Ngoc; Bounds, Richard; Zacharia, Anna; Itskos, Grigorios; Reimer, Jeffrey; Stylianou, Kyriakos; Chemical Science  (2019) –; doi:10.1039/C9SC01422E

data_1551056
_publ_section_title
;
 Temperature-dependent Interchromophoric Interaction in a Fluorescent
 Pyrene-based Metal--organic Framework
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01422E
_journal_year                    2019
_chemical_formula_moiety         'C88 H48 Mg3 O20'
_chemical_formula_sum            'C96.38 H67.56 Mg3 N2.79 O22.79'
_chemical_formula_weight         1702.28
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-02-13 deposited with the CCDC.    2019-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                80.439(3)
_cell_angle_beta                 77.037(4)
_cell_angle_gamma                75.856(3)
_cell_formula_units_Z            1
_cell_length_a                   11.4034(5)
_cell_length_b                   14.6274(5)
_cell_length_c                   16.1091(7)
_cell_measurement_reflns_used    4518
_cell_measurement_temperature    350
_cell_measurement_theta_max      30.9120
_cell_measurement_theta_min      1.8560
_cell_volume                     2521.50(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      350
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.751
_diffrn_measured_fraction_theta_max 0.571
_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      0.00 360.00   1.00    1.00    --    0.00   0.00   0.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  PILATUS@SNBL
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0126964000
_diffrn_orient_matrix_UB_12      0.0044435000
_diffrn_orient_matrix_UB_13      0.0404187000
_diffrn_orient_matrix_UB_21      -0.0492795000
_diffrn_orient_matrix_UB_22      -0.0225428000
_diffrn_orient_matrix_UB_23      0.0215559000
_diffrn_orient_matrix_UB_31      0.0417362000
_diffrn_orient_matrix_UB_32      -0.0452009000
_diffrn_orient_matrix_UB_33      -0.0007247000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0507
_diffrn_reflns_Laue_measured_fraction_full 0.751
_diffrn_reflns_Laue_measured_fraction_max 0.571
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18816
_diffrn_reflns_point_group_measured_fraction_full 0.751
_diffrn_reflns_point_group_measured_fraction_max 0.571
_diffrn_reflns_theta_full        25.374
_diffrn_reflns_theta_max         31.795
_diffrn_reflns_theta_min         1.886
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.238
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9688
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.238
_refine_ls_R_factor_all          0.1120
_refine_ls_R_factor_gt           0.1059
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3011
_refine_ls_wR_factor_ref         0.3093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8388
_reflns_number_total             9688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01422e2.cif
_cod_data_source_block           SION7_T350
_cod_original_cell_volume        2521.50(19)
_cod_database_code               1551056
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.983
_reflns_odcompleteness_completeness 57.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.80
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained planarity
 C51, C52, C53, C54, C55, C56
 with sigma of 0.1
 C31, C32, C33, C34, C35, C36
 with sigma of 0.1
3.a Rotating group:
 O2(H2A,H2B)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C22(H22), C23(H23),
 C25(H25), C26(H26), C32(H32), C33(H33), C35(H35), C36(H36), C42(H42), C43(H43),
  C45(H45), C46(H46), C52(H52), C53(H53), C55(H55), C56(H56)
;
_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 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.811