Crystalline arrays of molecular rotors with TIPS-trityl and phenolic-trityl stators using phenylene, 1,2-difluorophenylene and pyridine rotators
Arcos-Ramos, Rafael; Rodriguez-Molina, Braulio; Ramirez-Montes, Pedro; Gonzalez-Rodriguez, Edgar; Ochoa, Maria; Santillan, Rosa; Farfán, Norberto; Garcia-Garibay, Miguel A; RSC Adv.  (2015) –; doi:10.1039/C5RA07422C

data_7220774
_publ_section_title
;
 Crystalline arrays of molecular rotors with TIPS-trityl and
 phenolic-trityl stators using phenylene, 1,2-difluorophenylene and
 pyridine rotators
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA07422C
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C48 H34 O2, 2(C3 H6 O)'
_chemical_formula_sum            'C54 H46 O4'
_chemical_formula_weight         758.91
_chemical_name_common
;
1,4-bis-(([3-hydroxy-diphenyl]-phenylmethyl)-ethynyl)-phenylene acetone solvate
;
_chemical_name_systematic
;
1,4-bis-(([3-hydroxy-diphenyl]-phenylmethyl)-ethynyl)-phenylene acetone solvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-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     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2013-06-10
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2013-06-10 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                79.9847(17)
_cell_angle_beta                 74.7185(17)
_cell_angle_gamma                64.7483(19)
_cell_formula_units_Z            1
_cell_length_a                   8.95120(29)
_cell_length_b                   10.13470(40)
_cell_length_c                   13.22790(50)
_cell_measurement_reflns_used    4030
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_measurement_wavelength     0.71073
_cell_volume                     1044.36(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al, 2004)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.818
_diffrn_measured_fraction_theta_max 0.818
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.106816
_diffrn_orient_matrix_UB_12      -0.165368E-1
_diffrn_orient_matrix_UB_13      0.217713E-1
_diffrn_orient_matrix_UB_21      0.480902E-1
_diffrn_orient_matrix_UB_22      -0.760013E-1
_diffrn_orient_matrix_UB_23      0.552574E-1
_diffrn_orient_matrix_UB_31      -0.475106E-1
_diffrn_orient_matrix_UB_32      0.768871E-1
_diffrn_orient_matrix_UB_33      0.514289E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7523
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        29.15
_diffrn_reflns_theta_max         29.15
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.075
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.16(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4604
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.1387
_refine_ls_R_factor_gt           0.0826
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1370P)^2^+0.1737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2174
_refine_ls_wR_factor_ref         0.2512
_reflns_number_gt                2732
_reflns_number_total             4604
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra07422c2.cif
_cod_data_source_block           san183a
_cod_original_cell_volume        1044.358(69)
_cod_database_code               7220774