Solvatomorphism and Phase Transformation of CL-20: Probing Properties and Investigating Mechanisms
Pan, Bochen; Wang, Zhanzhong; Shen, Yichun; Wei, Liangxiao; Wei, Hongyuan; Dang, Leping; CrystEngComm  (2020) –; doi:10.1039/D0CE00059K

data_7240420
_publ_section_title
;
 Solvatomorphism and Phase Transformation of CL-20: Probing Properties and
 Investigating Mechanisms
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00059K
_journal_year                    2020
_chemical_formula_moiety         'C6 H6 N12 O12, 2(C4 H9 N O)'
_chemical_formula_sum            'C14 H24 N14 O14'
_chemical_formula_weight         612.47
_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   geom
_audit_creation_date             2019-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_audit_update_record
;
2019-07-20 deposited with the CCDC.	2020-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.25(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.344(3)
_cell_length_b                   8.2595(17)
_cell_length_c                   24.392(5)
_cell_measurement_reflns_used    6850
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8824
_cell_measurement_theta_min      1.5678
_cell_volume                     2616.8(10)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0503
_diffrn_reflns_av_unetI/netI     0.0736
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            29338
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.826
_diffrn_reflns_theta_min         1.605
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       prism
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 2251 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.1(8)
_refine_ls_extinction_coef       0.029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         12330
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      7.327
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0801P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1552
_reflns_Friedel_coverage         0.863
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                8012
_reflns_number_total             12330
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00059k2.cif
_cod_data_source_block           1905620
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7240420
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.973
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 N27-C23 = N27-C24 = N28-C26 = N28-C27 = N28-C28
 1.5 with sigma of 0.01
 N25-C14 = N25-C15 = N25-C16 = N26_$1-C18_$1 = N26_$1-C19_$1 = N26_$1-C20_$1
 1.5 with sigma of 0.01
 C13-C14 = C17_$1-C18_$1 = C25_$3-C26_$5
 1.54 with sigma of 0.01
 O25-C14 = O26_$1-C18_$1 = O28_$5-C26_$5
 1.22 with sigma of 0.01
 C15-C14A = C14-C13
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(N28) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(N27) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C16) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(C14A) = Uanis(C14)
Uanis(N25A) = Uanis(N25)
Uanis(C26A) = Uanis(C26)
Uanis(N28) = Uanis(N28A)
Uanis(N27A) = Uanis(N27)
Uanis(C22) = Uanis(C22A)
4. Others
 Sof(H13D)=Sof(H13E)=Sof(H13F)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(N25A)=1-FVAR(1)
 Sof(N25)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C14A)=1-FVAR(2)
 Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=FVAR(2)
 Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C26A)=1-FVAR(3)
 Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=FVAR(3)
 Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(N28A)=1-FVAR(4)
 Sof(N28)=Sof(H27A)=Sof(H27B)=Sof(H27C)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(4)
 Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(N27A)=1-FVAR(5)
 Sof(N27)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(H24A)=Sof(H24B)=Sof(H24C)=FVAR(5)
 Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C22A)=1-FVAR(6)
 Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=FVAR(6)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12)
5.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C13(H13D,H13E,H13F), C15(H15A,H15B,H15C), C15(H15D,H15E,
 H15F), C16(H16A,H16B,H16C), C16(H16D,H16E,H16F), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C21(H21D,H21E,H21F),
 C23(H23A,H23B,H23C), C23(H23D,H23E,H23F), C24(H24A,H24B,H24C), C24(H24D,H24E,
 H24F), C25(H25A,H25B,H25C), C25(H25D,H25E,H25F), C27(H27A,H27B,H27C), C27(H27D,
 H27E,H27F), C28(H28A,H28B,H28C), C28(H28D,H28E,H28F)
;
_shelx_res_checksum              94088
_shelx_hkl_checksum              94088
_olex2_submission_special_instructions 'No special instructions were received'