New High Pressure Crystal Structures of 2,2-Dimethylbutane and 2,3-Dimethylaniline: Combined X-ray, Raman, and Theoretical Studies
Bąk, Joanna M.; Gajda, Roman; Woźniak, Krzysztof; Crystal Growth & Design 15 (2015) 45–; doi:10.1021/cg500998g

data_4512517
_publ_section_title
;
 New High Pressure Crystal Structures of 2,2-Dimethylbutane and
 2,3-Dimethylaniline: Combined X-ray, Raman, and Theoretical Studies
;
_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              45
_journal_paper_doi               10.1021/cg500998g
_journal_volume                  15
_journal_year                    2015
_chemical_formula_moiety         'C8 H11 N'
_chemical_formula_sum            'C8 H11 N'
_chemical_formula_weight         121.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.871(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.1685(4)
_cell_length_b                   5.5274(3)
_cell_length_c                   12.422(4)
_cell_measurement_reflns_used    1495
_cell_measurement_temperature    293.(2)
_cell_measurement_theta_max      24.2120
_cell_measurement_theta_min      5.9520
_cell_volume                     348.51(12)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.(2)
_diffrn_measured_fraction_theta_full 0.267
_diffrn_measured_fraction_theta_max 0.213
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.267
_diffrn_reflns_Laue_measured_fraction_max 0.213
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3839
_diffrn_reflns_point_group_measured_fraction_full 0.273
_diffrn_reflns_point_group_measured_fraction_max 0.216
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         23.288
_diffrn_reflns_theta_min         4.321
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.068
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.365
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model (Absorb Angel (2004) J. Appl. Cryst. 37:486-492)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             132
_exptl_crystal_preparation       'mounted in a diamond-anvil cell '
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.055
_refine_diff_density_min         -0.041
_refine_diff_density_rms         0.012
_refine_ls_abs_structure_details
;
 Flack x determined using 148 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         445
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0347
_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^)+(0.0595P)^2^+0.0076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0840
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_full    0.280
_reflns_Friedel_fraction_max     0.219
_reflns_number_gt                362
_reflns_number_total             445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg500998g_si_001.cif
_cod_data_source_block           DMA
_cod_depositor_comments
'Adding full bibliography for 4512517--4512518.cif.'
_cod_original_cell_volume        348.50(12)
_cod_database_code               4512517
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C4 \\sim C8 \\sim C1 \\sim C2 \\sim C6 \\sim C5: within 1.7A with sigma of 0.02
and sigma for terminal atoms of 0.04
C7 \\sim C9 \\sim N3: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C6(H6)
3.b X=CH2 refined with riding coordinates:
 N3(H3A,H3B)
3.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              68856
_shelx_hkl_checksum              83040