Synthesis of Triptycene-Based Molecular Rotors for Langmuir-Blodgett Monolayers.
Kaleta, Jiří; Kaletová, Eva; Císařová, Ivana; Teat, Simon J.; Michl, Josef; The Journal of organic chemistry 80 (2015) 10134–10150; doi:10.1021/acs.joc.5b01753

data_4031548
_publ_section_title
;
 Synthesis of Triptycene-Based Molecular Rotors for Langmuir-Blodgett
 Monolayers.
;
_journal_issue                   20
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10134
_journal_page_last               10150
_journal_paper_doi               10.1021/acs.joc.5b01753
_journal_volume                  80
_journal_year                    2015
_chemical_compound_source        'synthesized by Dr. Jiri Kaleta'
_chemical_formula_moiety         'C57 H30 O2'
_chemical_formula_sum            'C71.5 H60 O5'
_chemical_formula_weight         999.19
_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   geom
_atom_sites_solution_primary     'Intrinsic Phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                97.056(7)
_cell_angle_beta                 92.982(6)
_cell_angle_gamma                100.618(7)
_cell_formula_units_Z            2
_cell_length_a                   8.1007(7)
_cell_length_b                   15.4383(14)
_cell_length_c                   22.617(2)
_cell_measurement_reflns_used    4129
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.65
_cell_measurement_theta_min      2.63
_cell_volume                     2750.9(4)
_computing_cell_refinement       'Bruker SAINT v8.34a'
_computing_data_collection       'Bruker APEX 2'
_computing_data_reduction        'Bruker SAINT v8.34a'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL & local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\w/\q shutterless scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.1249
_diffrn_reflns_av_unetI/netI     0.0666
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_number            4357
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        20.650
_diffrn_reflns_theta_max         20.668
_diffrn_reflns_theta_min         2.308
_diffrn_source                   'Advanced Light Source station 11.3.1'
_exptl_absorpt_coefficient_mu    0.088
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS 2012/1 Bruker AXS Madison WI USA'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       lath
_exptl_crystal_F_000             1058
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.883
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         4357
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.1384
_refine_ls_R_factor_gt           0.0960
_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          0.2689
_refine_ls_wR_factor_ref         0.3030
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2801
_reflns_number_total             4357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo5b01753_si_003.cif
_cod_data_source_block           JK566
_cod_depositor_comments
'Adding full bibliography for 4031540--4031548.cif.'
_cod_original_formula_sum        'C71.50 H60 O5'
_cod_database_code               4031548
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              97546
_shelx_hkl_checksum              48718