Thermal, spectroscopic and structural analysis of a thermosalient phase transformation in tapentadol hydrochloride
Gaztañaga, Pablo; Baggio, Ricardo; Halac, Emilia; Vega, Daniel R.; Acta Crystallographica Section B 75 (2019) –; doi:10.1107/S2052520619001148

data_2108381
_publ_section_title
;
 Thermal, spectroscopic and structural analysis of a thermosalient phase
 transformation in tapentadol hydrochloride
;
_journal_coeditor_code           LO5043SUP1
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520619001148
_journal_volume                  75
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C14 H24 N O, Cl'
_chemical_formula_sum            'C14 H24 Cl N O'
_chemical_formula_weight         257.79
_chemical_name_common            Tapentadol
_chemical_name_systematic
' (2R,3R)-3-(3-Hydroxyphenyl)-N,N,2-trimethylpentan-1-aminium '
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
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_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
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_cell_length_c                   17.4546(5)
_cell_measurement_reflns_used    7469
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      30.68
_cell_measurement_theta_min      2.92
_cell_volume                     1444.61(8)
_computing_cell_refinement       'Bruker SAINT'
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_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       11
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_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21544
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         35.170
_diffrn_reflns_theta_min         2.342
_exptl_absorpt_coefficient_mu    0.251
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_description       fragment
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_exptl_crystal_size_mid          0.18
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_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 3504 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         11785
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0543
_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^)+(0.0667P)^2^+0.3037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1360
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.880
_reflns_number_gt                9197
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_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_res_checksum              53182
_shelx_hkl_checksum              35939