4-Nitro-1-[(trimethylsilyl)ethynyl]benzene: low-temperature polymorph at 100K
Millican, Jasmine N.; Fronczek, Frank R.; Watkins, Steve F.; Acta Crystallographica Section E 68 (2012) o2652–; doi:10.1107/S1600536812034034

data_2236637
_publ_section_title
;
 4-Nitro-1-[(trimethylsilyl)ethynyl]benzene: low-temperature polymorph at
 100K
;
_journal_coeditor_code           SU2491
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2652
_journal_paper_doi               10.1107/S1600536812034034
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C11 H13 N1 O2 Si1'
_chemical_formula_moiety         'C11 H13 N1 O2 Si1'
_chemical_formula_sum            'C11 H13 N O2 Si'
_chemical_formula_weight         219.31
_chemical_name_systematic
;
4-Nitro-1-[(trimethylsilyl)ethynyl]benzene
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.222(2)
_cell_length_b                   7.128(2)
_cell_length_c                   16.537(4)
_cell_measurement_pressure       101.3
_cell_measurement_reflns_used    2709
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      34.3
_cell_measurement_theta_min      2.5
_cell_volume                     1204.9(5)
_computing_cell_refinement
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2002 (Burla <i>et al.</i>, 2003)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       ' \w and \f scans'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17805
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         33.75
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    0.176
_exptl_absorpt_correction_T_max  0.9792
_exptl_absorpt_correction_T_min  0.9657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'needle fragment'
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.317
_refine_ls_abs_structure_details 'Flack (1983), 1953 Bijvoet pairs'
_refine_ls_abs_structure_Flack   0.35(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     139
_refine_ls_number_reflns         4690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.4973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1229
_reflns_number_gt                3538
_reflns_number_total             4690
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su2491.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C11 H13 N1 O2 Si1'
_cod_database_code               2236637
_cod_database_fobs_code          2236637