A series of 4,5,9,10-tetrahydropyrene-based tetraarylethenes: synthesis, structures and solid-state emission behavior
Zhang, Zhao-Ming; Miao, Bao-Xi; Tang, Xin-Xue; Ni, Zhong-Hai; RSC Advances 8 (2018) 15173–; doi:10.1039/C8RA00057C

data_7230558
_publ_section_title
;
 A series of 4,5,9,10-tetrahydropyrene-based tetraarylethenes: synthesis,
 structures and solid-state emission behavior
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              15173
_journal_paper_doi               10.1039/C8RA00057C
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C56 H44'
_chemical_formula_sum            'C56 H44'
_chemical_formula_weight         716.91
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-05-09 deposited with the CCDC.
2018-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90.14(3)
_cell_angle_beta                 93.52(3)
_cell_angle_gamma                101.80(3)
_cell_formula_units_Z            2
_cell_length_a                   8.1823(16)
_cell_length_b                   12.694(3)
_cell_length_c                   19.994(4)
_cell_measurement_reflns_used    8230
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.6806
_cell_measurement_theta_min      3.0494
_cell_volume                     2028.7(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2001)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  XP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24928
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_T_max  0.892
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_platon_squeeze_details
;
In the refinement, the unit cell includes a large region of disordered 
solvent water molecule, which could not be modeled as discrete atomic sites. 
We employed PLATON/SQUEEZE program for the final refinement. 
The analysis shows that the void in the unit cell has a volume of 189.2 Ang^3. 
The residual electron density count amounts to 37 e per unit cell, 
corresponding to about one water molecule and one ethanol
molecule (0.5 water molecule and 0.5 ethanol
molecule per asymmetric unit). 

N: Total Potential Solvent Accessible Void Vol ..................   189.2 Ang^3
N: Electron Count / Cell =     37
;
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0874P)^2^+0.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2150
_reflns_number_gt                4032
_reflns_number_total             7079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ra00057c2.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        2028.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7230558