Piperazine-1,4-diol (PipzDiol): synthesis, stereodynamics and assembly of supramolecular hydrogen-bonded 2D networks
Lesnikov, Vladislav K.; Nelyubina, Yulia V.; Sukhorukov, Alexey Yu.; New Journal of Chemistry 46 (2022) 20386–20394; doi:10.1039/D2NJ03012H

data_7061962
_publ_section_title
;
 Piperazine-1,4-diol (PipzDiol): synthesis, stereodynamics and assembly of
 supramolecular hydrogen-bonded 2D networks
;
_journal_issue                   42
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              20386
_journal_page_last               20394
_journal_paper_doi               10.1039/D2NJ03012H
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'O4 S, 2(C2 H6 N O)'
_chemical_formula_sum            'C4 H12 N2 O6 S'
_chemical_formula_weight         216.22
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-10-10 downloaded from the CCDC.
;
_cell_angle_alpha                76.647(2)
_cell_angle_beta                 78.320(2)
_cell_angle_gamma                74.621(2)
_cell_formula_units_Z            2
_cell_length_a                   5.7797(4)
_cell_length_b                   6.3309(5)
_cell_length_c                   12.8187(10)
_cell_measurement_reflns_used    1764
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      3.30
_cell_volume                     435.01(6)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII DUO 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  0.0303
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         1.652
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0480 before and 0.0403 after correction.
The Ratio of minimum to maximum transmission is 0.9225.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_description       needle
_exptl_crystal_F_000             228
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         2302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0439P)^2^+0.1377P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1949
_reflns_number_total             2302
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03012h2.cif
_cod_data_source_block           LVK175
_cod_depositor_comments
'Adding full bibliography for 7061962--7061964.cif.'
_cod_database_code               7061962
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.879
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All O(H) groups
2.a Riding coordinates:
 O1(H1), N1(H1A), O2(H2), N2(H2C)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1B,H1C), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
;
_shelx_res_checksum              86449
_olex2_submission_special_instructions 'No special instructions were received'