Synthesis and crystal structure of a new polymorph of diisopropylammonium trichloroacetate, C8H16Cl3NO2
Reiss, Guido J.; Meyer, Michaela K.; Graf, Jürgen; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 875–879; doi:10.1515/ncrs-2019-0064

data_8105879
_publ_section_title
;
 Synthesis and crystal structure of a new polymorph of diisopropylammonium
 trichloroacetate, C8H16Cl3NO2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              875
_journal_page_last               879
_journal_paper_doi               10.1515/ncrs-2019-0064
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C2 Cl3 O2, C6 H16 N'
_chemical_formula_sum            'C8 H16 Cl3 N O2'
_chemical_formula_weight         264.57
_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'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90.593(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.1804(5)
_cell_length_b                   19.4133(10)
_cell_length_c                   13.9191(7)
_cell_measurement_reflns_used    9938
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.45
_cell_volume                     2480.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    DIAMOND
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0635
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            56285
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        29.000
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.800
_exptl_absorpt_coefficient_mu    0.716
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Bruker Apex2 software
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       needle
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.507
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
;
 Flack x determined using 4522 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         13160
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0605
_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^)+(0.0150P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1387
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                11276
_reflns_number_total             13160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0064_suppl.cif
_cod_data_source_block           notwin2
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               8105879
_shelx_estimated_absorpt_t_min   0.713
_shelx_estimated_absorpt_t_max   0.965
_shelx_res_checksum              89813
_shelx_hkl_checksum              66932
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n