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_1551055
_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            'C106 H96 Mg3 N6 O26'
_chemical_formula_weight         1942.81
_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                81.410(3)
_cell_angle_beta                 77.802(3)
_cell_angle_gamma                77.284(3)
_cell_formula_units_Z            1
_cell_length_a                   11.2723(4)
_cell_length_b                   14.4121(5)
_cell_length_c                   15.9112(5)
_cell_measurement_reflns_used    7652
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      31.9960
_cell_measurement_theta_min      2.0640
_cell_volume                     2450.19(15)
_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      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            PILATUS2M
_diffrn_measured_fraction_theta_full 0.751
_diffrn_measured_fraction_theta_max 0.569
_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      0.0144149000
_diffrn_orient_matrix_UB_12      0.0012335000
_diffrn_orient_matrix_UB_13      0.0413751000
_diffrn_orient_matrix_UB_21      -0.0463595000
_diffrn_orient_matrix_UB_22      -0.0272203000
_diffrn_orient_matrix_UB_23      0.0198156000
_diffrn_orient_matrix_UB_31      0.0448465000
_diffrn_orient_matrix_UB_32      -0.0432287000
_diffrn_orient_matrix_UB_33      -0.0054067000
_diffrn_radiation_monochromator  'Si (111)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7142
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.751
_diffrn_reflns_Laue_measured_fraction_max 0.569
_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            18468
_diffrn_reflns_point_group_measured_fraction_full 0.751
_diffrn_reflns_point_group_measured_fraction_max 0.569
_diffrn_reflns_theta_full        25.374
_diffrn_reflns_theta_max         31.973
_diffrn_reflns_theta_min         2.077
_diffrn_source
'European Synchrotron Radiation Facility, BM01 beamline'
_exptl_absorpt_coefficient_mu    0.112
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95437
_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    1.317
_exptl_crystal_description       block
_exptl_crystal_F_000             1018
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.499
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         9526
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1124P)^2^+2.7792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2070
_refine_ls_wR_factor_ref         0.2105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8956
_reflns_number_total             9526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01422e2.cif
_cod_data_source_block           SION7_T100
_cod_database_code               1551055
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.980
_reflns_odcompleteness_completeness 56.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.97
_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 1.095
_oxdiff_exptl_absorpt_empirical_full_min 0.905