Reversible facile single-crystal-to-single-crystal polymorphic transition accompanied by unit cell volume expansion and twinning
Wang, Kunlin; Wang, Chenguang; Mishra, Manish Kumar; Young, Victor G.; Sun, Changquan Calvin; CrystEngComm 23 (2021) 2648–2653; doi:10.1039/D1CE00055A

data_7242492
_publ_section_title
;
 Reversible facile single-crystal-to-single-crystal polymorphic transition
 accompanied by unit cell volume expansion and twinning
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2648
_journal_page_last               2653
_journal_paper_doi               10.1039/D1CE00055A
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C17 H22 N O, C6 H7 O7'
_chemical_formula_sum            'C23 H29 N O8'
_chemical_formula_weight         447.47
_chemical_melting_point          424
_chemical_name_common            'Diphenhydramine citrate salt'
_chemical_name_systematic
;
2-(Benzhydryloxy)-N,N-dimethylethanamine 2-hydroxypropane-1,2,3-tricarboxylate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-06-26 deposited with the CCDC.	2021-03-18 downloaded from the CCDC.
;
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_cell_angle_beta                 91.327(4)
_cell_angle_gamma                90
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_cell_length_c                   11.1075(10)
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_cell_measurement_temperature    218(2)
_cell_measurement_theta_max      30.38
_cell_measurement_theta_min      2.79
_cell_volume                     2279.5(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_diffrn_ambient_temperature      218(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker-AXS PHOTON-II CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.995
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_diffrn_reflns_point_group_measured_fraction_full 0.995
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_diffrn_reflns_theta_max         30.528
_diffrn_reflns_theta_min         2.879
_diffrn_source                   normal
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.7461
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2, (Sheldrick, 2015)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
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_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6778
_refine_diff_density_max         0.356
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         6900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.7187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1075
_refine_ls_wR_factor_ref         0.1159
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5694
_reflns_number_total             6900
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00055a2.cif
_cod_data_source_block           218k
_cod_depositor_comments
'Adding full bibliography for 7242491--7242493.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7242492
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.971
_shelx_estimated_absorpt_t_max   0.990
_shelx_res_checksum              97712
_shelx_hkl_checksum              55778