Mesoporous stilbene-based lanthanide metal organic frameworks: synthesis, photoluminescence and radioluminescence characteristics.
Mathis Ii, Stephan R.; Golafale, Saki T.; Bacsa, John; Steiner, Alexander; Ingram, Conrad W.; Doty, F. Patrick; Auden, Elizabeth; Hattar, Khalid; Dalton transactions (Cambridge, England : 2003) 46 (2017) 491–500; doi:10.1039/c6dt03755k

data_7041358
_publ_section_title
;
 Mesoporous stilbene-based lanthanide metal organic frameworks: synthesis,
 photoluminescence and radioluminescence characteristics.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              491
_journal_page_last               500
_journal_paper_doi               10.1039/c6dt03755k
_journal_volume                  46
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C64 H40 O21 Tm3'
_chemical_formula_sum            'C64 H40 O21 Tm3'
_chemical_formula_weight         1651.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-08-28
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_audit_update_record
;
2016-08-29 deposited with the CCDC.
2016-12-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 89.991(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.4920(8)
_cell_length_b                   15.9861(7)
_cell_length_c                   25.7022(13)
_cell_measurement_reflns_used    12210
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.6310
_cell_measurement_theta_min      2.0650
_cell_volume                     12528.5(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -60.65 127.35   0.50   30.00    --  -28.00  73.75 136.51  376
  2  \w    -60.65 127.35   0.50   30.00    --  -28.00  73.75   3.80  376
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Bruker D8 diffractometer with APEX2 detector'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0016148000
_diffrn_orient_matrix_UB_12      -0.0254418000
_diffrn_orient_matrix_UB_13      -0.0225403000
_diffrn_orient_matrix_UB_21      0.0199688000
_diffrn_orient_matrix_UB_22      0.0200059000
_diffrn_orient_matrix_UB_23      -0.0067300000
_diffrn_orient_matrix_UB_31      0.0118092000
_diffrn_orient_matrix_UB_32      -0.0303596000
_diffrn_orient_matrix_UB_33      0.0144476000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0404
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            34959
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.072
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_source_voltage           45
_exptl_absorpt_coefficient_mu    2.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.876
_exptl_crystal_description       prism
_exptl_crystal_F_000             3196
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.205
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.991
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.150
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         19378
_refine_ls_number_restraints     2125
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0914
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1262P)^2^+57.3098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1910
_refine_ls_wR_factor_ref         0.2053
_reflns_Friedel_coverage         0.999
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                15713
_reflns_number_total             19378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03755k2.cif
_cod_data_source_block           tmsdc_od_sq
_cod_depositor_comments
'Adding full bibliography for 7041358--7041359.cif.'
_cod_database_code               7041358
_chemical_oxdiff_formula         C27H37GaN6O6S3
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.641
_reflns_odcompleteness_completeness 99.30
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.29(3) 0.203(17) 0.265(19) 0.239(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
3. Restrained distances
 Tm3-O5
 2.34 with sigma of 0.05
 Tm1-O1
 2.34 with sigma of 0.05
 Tm2-O3
 2.34 with sigma of 0.02
 Tm2-O4
 2.34 with sigma of 0.02
 O3-O4
 2.5 with sigma of 0.02
 Tm2-O2
 2.34 with sigma of 0.05
 C18-C38_$1 \\sim C28-C88_$2 \\sim C48-C68_$2 \\sim C58-C78_$3
 with sigma of 0.02
 O5-O62 \\sim O5-O32_$4
 with sigma of 0.05
 O5-O52 \\sim O5-O81
 with sigma of 0.05
 O1-O12 \\sim O1-O41
 with sigma of 0.05
 O1-O22 \\sim O1-O72_$5
 with sigma of 0.05
 O3-O21 \\sim O4-O61
 with sigma of 0.02
 O3-O11 \\sim O3-O51 \\sim O4-O11 \\sim O4-O51
 with sigma of 0.02
 O2-O11 \\sim O2-O51
 with sigma of 0.02
 O2-O21 \\sim O2-O61
 with sigma of 0.02
4. Restrained planarity
 O11, O12, C11, C12, C13, C14, C15, C16, C17, C18
 with sigma of 0.005
 O21, O22, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma of 0.005
 O31, O32, C31, C32, C33, C34, C35, C36, C37, C38
 with sigma of 0.005
 O41, O42, C41, C42, C43, C44, C45, C46, C47, C48
 with sigma of 0.005
 O51, O52, C51, C52, C53, C54, C55, C56, C57, C58
 with sigma of 0.005
 O61, O62, C61, C62, C63, C64, C65, C66, C67, C68
 with sigma of 0.005
 O71, O72, C71, C72, C73, C74, C75, C76, C77, C78
 with sigma of 0.005
 O81, O82, C81, C82, C83, C84, C85, C86, C87, C88
 with sigma of 0.005
5. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
Uanis(C11) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C41) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C21) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(C31) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O1) \\sim Ueq: with sigma of 0.004 and sigma for terminal atoms of 0.008
Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.0045 and sigma for
terminal atoms of 0.009
Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C61) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(C81) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O1) = Uanis(O5)
Uanis(O3) = Uanis(O4)
6. Rigid body (RIGU) restrains
 O11, O12, C11, C12, C13, C14, C15, C16, C17, C18
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O41, O42, C41, C42, C43, C44, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O21, O22, C21, C22, C23, C24, C25, C26, C27, C28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O31, O32, C31, C32, C33, C34, C35, C36, C37, C38
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
7. Same fragment restrains
{O12, O11, C11, C12, C17, C16, C15, C14, C13, C18} sigma for 1-2: 0.005, 1-3:
0.04
{O21, O22, C21, C22, C23, C24, C25, C26, C27, C28} sigma for 1-2: 0.005, 1-3:
0.04
{O31, O32, C31, C32, C33, C34, C35, C36, C37, C38} sigma for 1-2: 0.005, 1-3:
0.04
{O41, O42, C41, C42, C43, C44, C45, C46, C47, C48} sigma for 1-2: 0.005, 1-3:
0.04
{O51, O52, C51, C52, C53, C54, C55, C56, C57, C58} sigma for 1-2: 0.005, 1-3:
0.04
{O61, O62, C61, C62, C63, C64, C65, C66, C67, C68} sigma for 1-2: 0.005, 1-3:
0.04
{O71, O72, C71, C72, C73, C74, C75, C76, C77, C78} sigma for 1-2: 0.005, 1-3:
0.04
{O81, O82, C81, C82, C83, C84, C85, C86, C87, C88} sigma for 1-2: 0.005, 1-3:
0.04
as
{O11, O12, C11, C12, C13, C14, C15, C16, C17, C18}
8.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C23(H23), C24(H24),
 C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38),
  C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C53(H53), C54(H54),
 C56(H56), C57(H57), C58(H58), C63(H63), C64(H64), C66(H66), C67(H67), C68(H68),
  C73(H73), C74(H74), C76(H76), C77(H77), C78(H78), C83(H83), C84(H84),
 C86(H86), C87(H87), C88(H88)
;
_shelx_fab_checksum              86207
_shelx_shelxl_version_number     2014/7
_olex2_submission_original_sample_id TmSDSC
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.813