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_7226747
_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, C12 H24 O6, H4 N'
_chemical_formula_sum            'C12 H28 Cl N O10'
_chemical_formula_weight         381.80
_chemical_name_common            AP/18C6
_chemical_name_systematic        cocrystal
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-26 deposited with the CCDC.
2016-10-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.257(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.9447(9)
_cell_length_b                   8.6823(3)
_cell_length_c                   22.5551(11)
_cell_measurement_reflns_used    7247
_cell_measurement_temperature    176.41(10)
_cell_measurement_theta_max      70.8130
_cell_measurement_theta_min      5.5560
_cell_volume                     3785.3(3)
_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      N~2~
_diffrn_ambient_temperature      176.41(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -30.00   70.00   1.0000    1.1600
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000   30.0000 100

  2 omega  -21.00   69.00   1.0000    1.1600
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000  -60.0000 90

  3 omega  -18.00   80.00   1.0000    4.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -38.0000   60.0000 98

  4 omega   33.00  123.00   1.0000    4.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000 -180.0000 90

  5 omega   23.00  111.00   1.0000    4.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -125.0000 -180.0000 88

  6 omega   33.00  123.00   1.0000    4.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000   30.0000 90

  7 omega  -15.00   75.00   1.0000    4.6400
omega____ theta____ kappa____ phi______ frames
    -       54.0000  -57.0000 -180.0000 90

  8 omega   35.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000    0.0000 58

  9 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -120.0000 96

 10 omega   35.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000   60.0000 58

 11 omega   36.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000 -180.0000 80

 12 omega   36.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 80

 13 omega   36.00  116.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000    0.0000 80

 14 omega   36.00   93.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 57

 15 omega   82.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   38.0000 -180.0000 96

 16 omega   40.00  130.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -63.0000   30.0000 90
;
_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      -0.0079816000
_diffrn_orient_matrix_UB_12      0.0113863000
_diffrn_orient_matrix_UB_13      0.0641559000
_diffrn_orient_matrix_UB_21      -0.0776764000
_diffrn_orient_matrix_UB_22      0.0343984000
_diffrn_orient_matrix_UB_23      -0.0432965000
_diffrn_orient_matrix_UB_31      -0.0159125000
_diffrn_orient_matrix_UB_32      -0.1736910000
_diffrn_orient_matrix_UB_33      -0.0043573000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20336
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.073
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         3.873
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59697
_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    1.340
_exptl_crystal_F_000             1632
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol/MTBE'
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         6762
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0970P)^2^+1.2160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1616
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5631
_reflns_number_total             6762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce01455k1.cif
_cod_data_source_block           xnkj-cmm-3
_cod_depositor_comments
;
Adding full bibliography for 7226745--7226747.cif.

2017-03-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(Cl O4), 2(C12 H24 O6), 2(H4 N)'
_cod_original_formula_sum        'C24 H56 Cl2 N2 O20'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     763.60
_cod_database_code               7226747
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 N00G-H00Z
 0.9 with sigma of 0.02
 N00G-HD
 0.82 with sigma of 0.02
3. Rigid bond restraints
 C011, C015
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C00U, C00X
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.001
4.a Secondary CH2 refined with riding coordinates:
 C00P(H00A,H00B), C00Q(H00C,H00D), C00R(H00E,H00F), C00S(H00G,H00H), C00T(H00I,
 H00J), C00V(H00K,H00L), C00W(H00M,H00N), C00X(H00S,H00T), C00Y(H00O,H00P),
 C00Z(H00U,H00V), C010(H01I,H01J), C011(H01A,H01B), C012(H01K,H01L), C013(H01C,
 H01D), C014(H01E,H01F), C016(H01M,H01N), C017(H01O,H01P), C018(H01Q,H01R),
 C019(H01S,H01T), C01A(H01U,H01V), C01B(H01W,H01X), C01C(H01Y,H)
;
_shelx_res_checksum              45287
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-07-01
_olex2_submission_special_instructions 'No special instructions were received'