Crystalline structure of an ammonia borane‒polyethylene oxide cocrystal: a material investigated for its hydrogen storage potential
Ploszajski, Anna R.; Billing, Matthew; Cockcroft, Jeremy K.; Skipper, Neal T.; CrystEngComm 20 (2018) 4436–; doi:10.1039/C8CE00872H

data_7231072
_publ_section_title
;
 Crystalline structure of an ammonia borane--polyethylene oxide cocrystal:
 a material investigated for its hydrogen storage potential
;
_journal_issue                   31
_journal_name_full               CrystEngComm
_journal_page_first              4436
_journal_paper_doi               10.1039/C8CE00872H
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C10 H20 O5, B H6 N'
_chemical_formula_sum            'C10 H26 B N O5'
_chemical_formula_weight         251.13
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.5852(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.42518(12)
_cell_length_b                   8.39871(16)
_cell_length_c                   20.2469(3)
_cell_measurement_reflns_used    11522
_cell_measurement_temperature    150.04(10)
_cell_measurement_theta_max      74.1580
_cell_measurement_theta_min      5.6130
_cell_volume                     1432.14(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      150.
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2031
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -39.00 -14.00   1.00    5.00    --  -42.62 -57.00  90.00   25
  2  \w    -61.00 -10.00   1.00    5.00    --  -42.62 -77.00   0.00   51
  3  \w    -44.00 -14.00   1.00    5.00    --  -42.62 -77.00 -60.00   30
  4  \w    -59.00 -10.00   1.00    5.00    --  -42.62 -77.00-120.00   49
  5  \w    -68.00 -18.00   1.00    5.00    --  -42.62 -38.00-120.00   50
  6  \w    -82.00 -55.00   1.00    5.00    --  -42.62 -57.00  90.00   27
  7  \w    -99.00 -72.00   1.00    5.00    --  -42.62 -77.00   0.00   27
  8  \w   -119.00 -85.00   1.00    5.00    --  -42.62 -77.00 -60.00   34
  9  \w   -118.00 -71.00   1.00    5.00    --  -42.62 -77.00-120.00   47
 10  \w   -119.00 -10.00   1.00    5.00    --  -42.62 -77.00-180.00  109
 11  \w      2.00  50.00   1.00    5.00    --   42.62 -99.00 -60.00   48
 12  \w     23.00  98.00   1.00    5.00    --   42.62-125.00  30.00   75
 13  \w     32.00 138.00   1.00   30.00    --  107.94 -77.00  60.00  106
 14  \w     79.00 160.00   1.00   30.00    --  107.94  61.00 -30.00   81
 15  \w    115.00 142.00   1.00   30.00    --  107.94  77.00-150.00   27
 16  \w     79.00 123.00   1.00   30.00    --  107.94  61.00 -90.00   44
 17  \w     76.00 167.00   1.00   30.00    --  107.94  77.00-180.00   91
 18  \w     79.00 110.00   1.00   30.00    --  107.94  61.00-150.00   31
 19  \w     75.00 177.00   1.00   30.00    --  107.94  77.00 -90.00  102
 20  \w    115.00 178.00   1.00   30.00    --  107.94  77.00  90.00   63
 21  \w    114.00 178.00   1.00   30.00    --  107.94  77.00 120.00   64
 22  \w     81.00 145.00   1.00   30.00    --  107.94  55.00 174.43   64
 23  \w     80.00 105.00   1.00   30.00    --  107.94  61.00  60.00   25
 24  \w     77.00 103.00   1.00   30.00    --  107.94  70.00  29.82   26
 25  \w     75.00 101.00   1.00   30.00    --  107.94  77.00  30.00   26
 26  \w     79.00 109.00   1.00   30.00    --  107.94  61.00   0.00   30
 27  \w     75.00 101.00   1.00   30.00    --  107.94  77.00  60.00   26
 28  \w     79.00 150.00   1.00   30.00    --  107.94  68.00  62.83   71
 29  \w     79.00 107.00   1.00   30.00    --  107.94  61.00 150.00   28
 30  \w     80.00 108.00   1.00   30.00    --  107.94  58.00 125.12   28
 31  \w     75.00 101.00   1.00   30.00    --  107.94  77.00 120.00   26
 32  \w     76.00 103.00   1.00   30.00    --  107.94  73.00 162.96   27
 33  \w     75.00 101.00   1.00   30.00    --  107.94  77.00  90.00   26
 34  \w     77.00 103.00   1.00   30.00    --  107.94  70.00  87.57   26
 35  \w     75.00 143.00   1.00   30.00    --  107.94  77.00   0.00   68
 36  \w     79.00 176.00   1.00   30.00    --  107.94  61.00-120.00   97
 37  \w     82.00 173.00   1.00   30.00    --  107.94 146.00  -6.00   91
 38  \w     76.00 102.00   1.00   30.00    --  107.94  75.00-127.28   26
 39  \w     75.00 101.00   1.00   30.00    --  107.94  77.00-120.00   26
 40  \w     75.00 102.00   1.00   30.00    --  107.94  77.00-150.00   27
 41  \w     76.00 104.00   1.00   30.00    --  107.94  74.00 -76.61   28
 42  \w     75.00 102.00   1.00   30.00    --  107.94  77.00 -60.00   27
 43  \w     75.00 178.00   1.00   30.00    --  107.94  77.00 -30.00  103
 44  \w     23.00  74.00   1.00    5.00    --   42.62-125.00 109.00   51
 45  \w     32.00 108.00   1.00   30.00    --  107.94 -95.00  30.00   76
 46  \w     26.00 104.00   1.00   30.00    --  107.94 -95.00 -60.00   78
 47  \w    -70.00  31.00   1.00    5.00    --  -42.62  57.00-150.00  101
 48  \w   -116.00 -12.00   1.00    5.00    --  -42.62 -77.00  90.00  104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0959724000
_diffrn_orient_matrix_UB_12      -0.0298225000
_diffrn_orient_matrix_UB_13      -0.0647124000
_diffrn_orient_matrix_UB_21      -0.1515008000
_diffrn_orient_matrix_UB_22      -0.0232435000
_diffrn_orient_matrix_UB_23      0.0396855000
_diffrn_orient_matrix_UB_31      -0.0352321000
_diffrn_orient_matrix_UB_32      0.1796470000
_diffrn_orient_matrix_UB_33      -0.0056156000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0134
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21539
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.408
_diffrn_reflns_theta_min         4.369
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.740
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_description       plate
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.317
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.024
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     156
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0587
_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^)+(0.0920P)^2^+0.7906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1684
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2622
_reflns_number_total             2909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce00872h2.cif
_cod_data_source_block           xstr0748
_cod_depositor_comments
'Adding full bibliography for 7231072--7231073.cif.'
_cod_original_cell_volume        1432.13(4)
_cod_database_code               7231072
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C10 H26 B N O5'
_chemical_oxdiff_usercomment     'Sample left for 10 months'
_reflns_odcompleteness_completeness 99.96
_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
 At 1.5 times of:
  All B(H,H,H) groups, All N(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B)
2.b Idealised Me refined as rotating group:
 N1(H1C,H1D,H1E), B1(H1F,H1G,H1H)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.398
_oxdiff_exptl_absorpt_empirical_full_min 0.777