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_7220772
_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         'C66 H72 F2 O2 Si2'
_chemical_formula_sum            'C66 H72 F2 O2 Si2'
_chemical_formula_weight         991.42
_chemical_name_common
;
1,4-bis[(3,3,-diphenyl-3-(3?-(tri-isopropylsylanoxy)-phenyl)-prop-1-yn-1-yl)]-2,3-difluorobenzene'
;
_chemical_name_systematic
;
1,4-bis[(3,3,-diphenyl-3-(3?-(tri-isopropylsylanoxy)-phenyl)-prop-1-yn-1-yl)]-2,3-difluorobenzene
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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             2013-06-05
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2013-06-08 deposited with the CCDC.
2015-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   25.02220(50)
_cell_length_b                   29.77010(50)
_cell_length_c                   7.49480(10)
_cell_measurement_reflns_used    44750
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_measurement_wavelength     0.71073
_cell_volume                     5582.98(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_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      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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 Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.74309E-2
_diffrn_orient_matrix_UB_12      0.122964E-1
_diffrn_orient_matrix_UB_13      0.319064E-1
_diffrn_orient_matrix_UB_21      0.672499E-1
_diffrn_orient_matrix_UB_22      0.324735E-1
_diffrn_orient_matrix_UB_23      -0.9834E-2
_diffrn_orient_matrix_UB_31      -0.114999
_diffrn_orient_matrix_UB_32      0.197847E-1
_diffrn_orient_matrix_UB_33      -0.36891E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            44573
_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        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.114
_exptl_absorpt_correction_T_max  1.0328
_exptl_absorpt_correction_T_min  0.9024
_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    1.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.462
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0054(12)
_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   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6385
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1799
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1237P)^2^+9.3189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2273
_refine_ls_wR_factor_ref         0.2778
_reflns_number_gt                3446
_reflns_number_total             6385
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c5ra07422c2.cif
_cod_data_source_block           san649x
_cod_original_cell_volume        5582.977(163)
_cod_database_code               7220772