Polymorphism and structural diversities of LiClO4 - β-alanine ionic co-crystals
Marek, Paulina Halina; Cichowicz, Grzegorz; Osowicka, Dorota; Madura, Izabela Dorota; Dobrzycki, Lukasz; Cyranski, Michal; Ciesielski, Arkadiusz; CrystEngComm  (2020) –; doi:10.1039/D0CE00592D

data_7240566
_publ_section_title
;
 Polymorphism and structural diversities of LiClO4 - \b-alanine ionic
 co-crystals
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00592D
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C6 H14 Li N2 O4, Cl O4'
_chemical_formula_sum            'C6 H14 Cl Li N2 O8'
_chemical_formula_weight         284.58
_chemical_name_systematic
'catena-(bis(/m-2-beta-Alanine)-lithium perchlorate)'
_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   mixed
_audit_creation_date             2019-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-08 deposited with the CCDC.	2020-05-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.899(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.9667(6)
_cell_length_b                   8.4410(11)
_cell_length_c                   13.9410(18)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.41
_cell_volume                     581.37(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker Nano, Inc., 2016)'
_computing_data_collection       'APEX3 V2019 (Bruker Nano, Inc., 2019)'
_computing_data_reduction        'SAINT V8.38A (Bruker Nano, Inc., 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\o and \f scans'
_diffrn_radiation_monochromator  TRIUMPH
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17343
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         2.83
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6959
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0731 before and 0.0675 after correction.
The Ratio of minimum to maximum transmission is 0.9327.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             296
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.291
_refine_ls_abs_structure_details
;

Flack x determined using 1576 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3541
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0313P)^2^+0.0991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0648
_reflns_number_gt                3477
_reflns_number_total             3541
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00592d2.cif
_cod_data_source_block           2
_cod_database_code               7240566
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.902
_shelx_res_checksum              96543