Part 2. Structures of 4-trimethylsilylethynyl-<i>N</i>,<i>N</i>-dimethylaniline, and 4-ethynyl-<i>N</i>,<i>N</i>-dimethylaniline with <i>Z</i>′ = 12 and a single-crystal to single-crystal phase transition at 122.5 ± 2 K
Andrei S. Batsanov; Jonathan C. Collings; Richard M. Ward; Andrés E. Goeta; Laurent Porrès; Andrew Beeby; Judith A. K. Howard; Jonathan W. Steed; Todd B. Marder; CrystEngComm 8 (2006) 622–; doi:10.1039/b606327f

data_7203447
_publ_section_title
;
 Part 2. Structures of
 4-trimethylsilylethynyl-<i>N</i>,<i>N</i>-dimethylaniline, and
 4-ethynyl-<i>N</i>,<i>N</i>-dimethylaniline with <i>Z</i>&#x2032;                =
 12 and a single-crystal to single-crystal phase transition at 122.5 +-
 2 K
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              622
_journal_paper_doi               10.1039/b606327f
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C10 H11 N'
_chemical_formula_sum            'C10 H11 N'
_chemical_formula_weight         145.20
_chemical_melting_point          310.5(5)
_chemical_name_common            (4-ethynyl-phenyl)-dimethyl-amine
_chemical_name_systematic
;
(4-ethynyl-phenyl)-dimethyl-amine
;
_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
_cell_angle_alpha                105.84(1)
_cell_angle_beta                 104.51(1)
_cell_angle_gamma                112.99(1)
_cell_formula_units_Z            24
_cell_length_a                   17.412(1)
_cell_length_b                   18.845(1)
_cell_length_c                   19.252(1)
_cell_measurement_reflns_used    3211
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.4
_cell_volume                     5119.4(10)
_computing_cell_refinement       'SAINT version 6.28A (Bruker, 2002)'
_computing_data_collection       'SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT version 6.28A (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL version 6.12 (Bruker, 2001)'
_computing_publication_material  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL version 6.12 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL version 6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ProteumM APEX CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source
'60W microfocus Bede Microsource with glass polycapillary optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_av_sigmaI/netI    0.1070
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            56475
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.79
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.216
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.912
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1285
_refine_ls_number_reflns         23457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.1749
_refine_ls_R_factor_gt           0.0585
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1481
_reflns_number_gt                9236
_reflns_number_total             23457
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b606327f.txt
_cod_data_source_block           \b-1
_cod_database_code               7203447