Crystal structure of guanidinium tetrapropylammonium bis(hydrogencarbonate) dihydrate, C15H40N4O8
Zeng, Huahui; Shen, Qianjin; Wu, Xiangxiang; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 1015–1017; doi:10.1515/ncrs-2018-0142

data_8106382
_publ_section_title
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 Crystal structure of guanidinium tetrapropylammonium
 bis(hydrogencarbonate) dihydrate, C15H40N4O8
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_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1015
_journal_page_last               1017
_journal_paper_doi               10.1515/ncrs-2018-0142
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         '0.5(C16 H12 Br2 F2 O4 S2)'
_chemical_formula_sum            'C8 H6 Br F O2 S'
_chemical_formula_weight         265.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 103.1370(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.7846(2)
_cell_length_b                   9.6099(4)
_cell_length_c                   10.3260(4)
_cell_measurement_reflns_used    5240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.30
_cell_measurement_theta_min      2.93
_cell_volume                     462.36(3)
_computing_cell_refinement       'SAINT-plus (Bruker, 2008 [8])'
_computing_data_collection       'APEX2 (Bruker, 2008 [7])'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker,2008 [9])'
_computing_molecular_graphics    'ORTEP-3 [12]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[11]'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)[10]'
_computing_structure_solution    'SHELXL-2016/4 (Sheldrick, 2016 [10])'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6634
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.295
_diffrn_reflns_theta_min         2.025
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.648
_exptl_absorpt_correction_T_max  0.522
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_meas      .
_exptl_crystal_description       rod
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.223
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0094(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1090
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0193
_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^)+(0.0246P)^2^+0.1282P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0494
_refine_ls_wR_factor_ref         0.0502
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1012
_reflns_number_total             1090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0142_suppl.cif
_cod_data_source_block           17zs
_cod_database_code               8106382
_shelx_estimated_absorpt_t_max   0.562
_shelx_estimated_absorpt_t_min   0.442
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C7 \\sim C7-C8 \\sim C8-C3
 with sigma of 0.02
 C3-C7 \\sim C3-C7 \\sim C6-C4 \\sim C6-C8 \\sim C8-C4 \\sim C7-C5
 with sigma of 0.04
3. Restrained planarity
 C3, C4, C5, C6, C7, C8
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08
Uanis(C7) = Uanis(C3)
Uanis(C4) = Uanis(C6)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: Br1(0.5) C2(0.5) H2(0.5) C1(0.5) H1(0.5) F1(0.5) C3(0.5) H3(0.5)
 C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5) H7(0.5) C8(0.5) O1(0.5) O2(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C1(H1), C3(H3), C4(H4), C6(H6), C7(H7)
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_shelx_res_checksum              65011
_shelx_hkl_checksum              38807
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
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