Cocrystals of ammonium perchlorate with a series of crown ethers: preparation, structures, and properties
Cheng, Minmin; Liu, Xun; Luo, Qingping; Duan, Xiaohui; Pei, Chonghua; CrystEngComm 18 (2016) 8487–; doi:10.1039/C6CE01455K

data_7226746
_publ_section_title
;
 Cocrystals of ammonium perchlorate with a series of crown ethers:
 preparation, structures, and properties
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              8487
_journal_paper_doi               10.1039/C6CE01455K
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'Cl O4, 1.5(C20 H24 O6), H4 N'
_chemical_formula_sum            'C30 H40 Cl N O13'
_chemical_formula_weight         658.08
_chemical_melting_point          470.65
_chemical_name_systematic        'AP/DB18C6 cocrystal'
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-09-01 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.3603(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6348(2)
_cell_length_b                   12.9180(2)
_cell_length_c                   20.7752(3)
_cell_measurement_reflns_used    8264
_cell_measurement_temperature    294.39(10)
_cell_measurement_theta_max      72.3030
_cell_measurement_theta_min      4.8080
_cell_volume                     3236.39(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.39(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_details
;
  1 omega  -31.00   53.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000    0.0000 84

  2 omega   20.00  104.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -180.0000 84

  3 omega   20.00  104.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   60.0000 84

  4 omega  -31.00   53.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000   30.0000 84

  5 omega   20.00  104.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -120.0000 84

  6 omega    7.00  108.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421   19.0000 -180.0000 101

  7 omega   23.00   90.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000  -30.0000 67

  8 omega   23.00   90.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -150.0000 67

  9 omega    1.00   75.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000   90.0000 74

 10 omega  -31.00   53.00   1.0000    3.0100
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  -60.0000 84

 11 omega   38.00   91.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   60.0000 53

 12 omega   38.00   91.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 13 omega   38.00   91.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

 14 omega   40.00   98.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -180.0000 58

 15 omega   39.00  109.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 16 omega   40.00  135.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   60.0000 95

 17 omega   38.00  116.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  150.0000 78

 18 omega   40.00   98.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 58

 19 omega   40.00   98.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 58

 20 omega   39.00   64.00   1.0000   12.0400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -150.0000 25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1136508000
_diffrn_orient_matrix_UB_12      0.0130282000
_diffrn_orient_matrix_UB_13      -0.0122830000
_diffrn_orient_matrix_UB_21      -0.0338226000
_diffrn_orient_matrix_UB_22      -0.0796560000
_diffrn_orient_matrix_UB_23      -0.0577442000
_diffrn_orient_matrix_UB_31      -0.0475187000
_diffrn_orient_matrix_UB_32      0.0877588000
_diffrn_orient_matrix_UB_33      -0.0505278000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0216
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19153
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.051
_diffrn_reflns_theta_max         67.051
_diffrn_reflns_theta_min         5.017
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.618
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66423
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       rod-like
_exptl_crystal_F_000             1392
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: N, N-dimethylformamide/methyl tert-butyl ether'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.067
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0823
_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^)+(0.1769P)^2^+1.6310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.2600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4734
_reflns_number_total             5551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01455k1.cif
_cod_data_source_block           xnkd-11-13-02
_cod_depositor_comments
'Adding full bibliography for 7226745--7226747.cif.'
_cod_original_cell_volume        3236.38(9)
_cod_database_code               7226746
_reflns_odcompleteness_completeness 95.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H) groups
2. Restrained distances
 N00B-HB
 0.85 with sigma of 0.01
3.a Free rotating group:
 N00B(H0AA,H)
3.b Secondary CH2 refined with riding coordinates:
 C00H(H00A,H00B), C00K(H00C,H00D), C00L(H00E,H00F), C00P(H00G,H00H), C00Q(H00Q,
 H00T), C00T(H00U,H00W), C00U(H00X,H00Y), C00W(H00I,H00J), C00X(H00,HC),
 C00Y(H00K,H00L), C013(H01A,H01B), C014(H01C,H01D)
3.c Aromatic/amide H refined with riding coordinates:
 C00I(H00P), C00M(H00M), C00N(H00N), C00O(H00O), C00R(H00R), C00S(H00S),
 C00V(H00V), C00Z(H00Z), C010(H010), C012(H012), C015(H015), C018(H018)
;
_shelx_res_checksum              14842
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-11-13
_olex2_submission_special_instructions 'No special instructions were received'