Role of crystallization water molecules on hydrogen-bonded structures and dielectric phase transitions in amino trimethylene phosphonic acid-based crystals
Sun, Yu-Ling; Zheng, Bei-Bei; Zhang, Wen; New J. Chem. 41 (2017) 5142–5150; doi:10.1039/C7NJ00612H

data_7056185
_publ_section_title
;
 Role of crystallization water molecules on hydrogen-bonded structures and
 dielectric phase transitions in amino trimethylene phosphonic acid-based
 crystals
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              5142
_journal_page_last               5150
_journal_paper_doi               10.1039/C7NJ00612H
_journal_volume                  41
_journal_year                    2017
_chemical_formula_moiety
'C6 H17 N2 O18 P6, 6(C4 H12 N), H3 O, 2(H2 O) '
_chemical_formula_sum            'C30 H96 N8 O21 P6'
_chemical_formula_weight         1090.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-12 deposited with the CCDC.
2017-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                103.678(9)
_cell_angle_beta                 99.604(5)
_cell_angle_gamma                102.404(11)
_cell_formula_units_Z            1
_cell_length_a                   11.474(9)
_cell_length_b                   11.641(9)
_cell_length_c                   11.834(9)
_cell_measurement_reflns_used    4119
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.5010
_cell_measurement_theta_min      3.6409
_cell_volume                     1460(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15579
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         3.591
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku, 2005)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       Prism
_exptl_crystal_F_000             590
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.298
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         6563
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      11.398
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0666P)^2^+0.3809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1241
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5537
_reflns_number_total             6563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nj00612h2.cif
_cod_data_source_block           2-273K
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7056185
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              87852